{"id":45300,"date":"2021-03-03T00:00:00","date_gmt":"2021-03-03T00:00:00","guid":{"rendered":"https:\/\/discover.restek.com\/uncategorized\/analyse-de-pesticides-mycotoxines-et-cannabinoides-dans-les-bonbons-gelifies-au-cannabis\/"},"modified":"2026-01-28T19:12:28","modified_gmt":"2026-01-28T19:12:28","slug":"analyse-de-pesticides-mycotoxines-et-cannabinoides-dans-les-bonbons-gelifies-au-cannabis","status":"publish","type":"post","link":"https:\/\/discover.restek.com\/fr\/notes-dapplication\/ffan3481-fr\/analyse-de-pesticides-mycotoxines-et-cannabinoides-dans-les-bonbons-gelifies-au-cannabis","title":{"rendered":"Analyse de pesticides, mycotoxines et cannabino\u00efdes dans les bonbons g\u00e9lifi\u00e9s au cannabis"},"content":{"rendered":"\n

R\u00e9sum\u00e9<\/h2>\n\n\n\n

L’\u00c9tat de Californie exige l\u2019analyse des pesticides, des mycotoxines et des cannabino\u00efdes dans tous les types de produits d\u00e9riv\u00e9s du cannabis [1]. Pour cette raison, il est n\u00e9cessaire de d\u00e9velopper des m\u00e9thodes fiables pour la quantification de ces analytes dans diverses matrices. Les bonbons g\u00e9lifi\u00e9s au cannabis sont un aliment tr\u00e8s populaire, mais leur composition en fait des matrices tr\u00e8s complexes. Dans cet article, nous d\u00e9crivons une m\u00e9thode d\u2019analyse de pesticides, mycotoxines et cannabino\u00efdes dans les bonbons g\u00e9lifi\u00e9s au cannabis, avec une simple et unique proc\u00e9dure d\u2019extraction.<\/p>\n\n\n\n

Introduction<\/h2>\n\n\n\n

Les produits comestibles infus\u00e9s de cannabis ou de cannabidiol (CBD) gagnent en popularit\u00e9 aupr\u00e8s des consommateurs de cannabis. En termes de tests, l\u2019analyse de la puissance de ces produits est obligatoire dans tous les \u00e9tats o\u00f9 les tests en laboratoire sont requis. De plus, dans l\u2019\u00c9tat de Californie, la d\u00e9termination des contaminants, comme les pesticides et les mycotoxines, dans les produits comestibles et autres produits d\u00e9riv\u00e9s du cannabis, est \u00e9galement une exigence. De par la grande vari\u00e9t\u00e9 de produits comestibles disponibles sur le march\u00e9, diff\u00e9rents strat\u00e9gies analytiques doivent \u00eatre suivies afin d\u2019obtenir des donn\u00e9es analytiques fiables pour tous les analytes d\u2019int\u00e9r\u00eat dans toutes les matrices. Parmi les diff\u00e9rents types de produits comestibles au cannabis, les bonbons g\u00e9lifi\u00e9s offrent des d\u00e9fis uniques aux laboratoires d\u2019analyse.<\/p>\n\n\n\n

Les bonbons g\u00e9lifi\u00e9s sont des matrices \u201ccollantes\u201d, g\u00e9n\u00e9ralement compos\u00e9s d\u2019ingr\u00e9dients tels que le sucre, l\u2019amidon, la pectine et la g\u00e9latine. En raison de leur composition, les strat\u00e9gies de pr\u00e9paration d\u2019\u00e9chantillons pour les analyses de puissance comprennent g\u00e9n\u00e9ralement une \u00e9tape de solubilisation des \u00e9chantillons dans des solvants comme l\u2019eau ou le DMSO, mais de larges volumes de solvant comme le m\u00e9thanol peuvent \u00e9galement \u00eatre utilis\u00e9s. Apr\u00e8s homog\u00e9n\u00e9isation des \u00e9chantillons, les cannabino\u00efdes sont quantifi\u00e9s par HPLC-UV, par injection soit des \u00e9chantillons extraits dilu\u00e9s, soit des \u00e9chantillons apr\u00e8s traitement par des sels QuEChERS. Les informations accessibles au public sont rares et limit\u00e9es en ce qui concerne l\u2019analyse de contaminants tels que les pesticides ou les mycotoxines dans les matrices telles que les bonbons g\u00e9lifi\u00e9s, avec un seul rapport montrant des donn\u00e9es semi-quantitatives pour 35 pesticides en utilisant la technique QuEChERS [2]. <\/p>\n\n\n\n

Dans cet article, nous proposons une m\u00e9thode robuste pour la quantification de la liste californienne de pesticides, mycotoxines et cannabino\u00efdes, dans des \u00e9chantillons de bonbons g\u00e9lifi\u00e9s. La m\u00e9thodologie de pr\u00e9paration des \u00e9chantillons a \u00e9t\u00e9 optimis\u00e9e, et implique une \u00e9tape de solubilisation, suivie d\u2019une \u00e9tape d\u2019extraction \u00e0 l\u2019ac\u00e9tonitrile acidifi\u00e9 puis d\u2019une \u00e9tape de dessalage \u00e0 l\u2019aide de sels QuEChERS EN. Pour l\u2019analyse des cannabino\u00efdes et autres contaminants analysables par LC, une simple dilution a \u00e9t\u00e9 effectu\u00e9e avant l\u2019injection. Pour les pesticides analysables par GC, l\u2019utilisation d\u2019un support dSPE compos\u00e9 d\u2019amine primaire\/secondaire (PSA), de noir de carbone graphite (GCB) et de sulfate de magn\u00e9sium a \u00e9t\u00e9 n\u00e9cessaire avant l\u2019analyse. Dans son ensemble, la m\u00e9thode propos\u00e9e pour l\u2019analyse de pesticides, mycotoxines et cannabino\u00efdes dans les bonbons g\u00e9lifi\u00e9s au cannabis fournit des r\u00e9sultats satisfaisants en termes de lin\u00e9arit\u00e9, d\u2019exactitude, de pr\u00e9cision et de limites de quantification (LOQ). <\/p>\n\n\n\n

M\u00e9thode<\/h2>\n\n\n\n

Pr\u00e9paration d’\u00e9chantillons<\/h3>\n\n\n\n

Apr\u00e8s de nombreux tests pr\u00e9liminaires de diff\u00e9rents param\u00e8tres exp\u00e9rimentaux, la m\u00e9thode suivante a \u00e9t\u00e9 mise en \u0153uvre (Figure 1). Les bonbons g\u00e9lifi\u00e9s ont \u00e9t\u00e9 hach\u00e9s puis pes\u00e9s (1 g) dans un tube de 50 mL (r\u00e9f. 25846), dans lequel 5 mL d\u2019eau ont \u00e9t\u00e9 ajout\u00e9s. Ensuite, les \u00e9chantillons ont \u00e9t\u00e9 pass\u00e9s au vortex, \u00e0 haute vitesse, jusqu\u2019\u00e0 ce que tous les morceaux de bonbons g\u00e9lifi\u00e9s soient solubilis\u00e9s. La solution a ensuite \u00e9t\u00e9 dop\u00e9e avec les analytes cibles et\/ou les standards internes (les standards internes n\u2019ont \u00e9t\u00e9 utilis\u00e9s que pour l\u2019analyse des contaminants, pas pour les analyses de puissance) et pass\u00e9e au vortex \u00e0 nouveau pendant 30 secondes. Ensuite, 5 mL d\u2019ac\u00e9tonitrile acidifi\u00e9 (avec de l\u2019acide ac\u00e9tique \u2013 1% v:v) ont \u00e9t\u00e9 ajout\u00e9s puis les \u00e9chantillons ont \u00e9t\u00e9 pass\u00e9s au vortex pour 30 secondes suppl\u00e9mentaires. Des sels d\u2019extraction QuEChERS Q-sep EN 15662 (r\u00e9f. 25849) ont ensuite \u00e9t\u00e9 ajout\u00e9s et les \u00e9chantillons ont \u00e9t\u00e9 pass\u00e9s \u00e0 nouveau au vortex puis centrifug\u00e9s pendant 5 minutes.<\/p>\n\n\n\n

Pour les analyses de puissance, 100 \u00b5L d\u2019\u00e9chantillon extrait ont \u00e9t\u00e9 m\u00e9lang\u00e9s avec 900 \u00b5L d\u2019une solution eau\/ac\u00e9tonitrile 25\/75, et 2 \u00b5L de la solution ainsi pr\u00e9par\u00e9e ont \u00e9t\u00e9 inject\u00e9s pour analyse par LC-UV. Pour les contaminants analysables par LC, 750 \u00b5L d\u2019\u00e9chantillon extrait ont \u00e9t\u00e9 m\u00e9lang\u00e9s avec 250 \u00b5L d\u2019eau, et 2 \u00b5L de la solution ainsi pr\u00e9par\u00e9e ont \u00e9t\u00e9 inject\u00e9s pour analyse par LC-MS\/MS. Pour les contaminants analysables par GC, 1.9 mL de l\u2019extrait ont \u00e9t\u00e9 transf\u00e9r\u00e9s dans un tube dSPE QuEChERS Q-sep contenant un m\u00e9lange de PSA, GCB et sulfate de magn\u00e9sium (r\u00e9f. 26217). Apr\u00e8s \u00eatre pass\u00e9s au vortex puis centrifug\u00e9s, 500 \u00b5L d\u2019extrait ont \u00e9t\u00e9 m\u00e9lang\u00e9s avec 500 \u00b5L d\u2019acide ac\u00e9tique \u00e0 1% dans l\u2019ac\u00e9tonitrile, et 1 \u00b5L de la solution ainsi pr\u00e9par\u00e9e a \u00e9t\u00e9 inject\u00e9 pour analyse par GC-MS\/MS.<\/p>\n\n\n

Figure 1 :<\/strong>\u00a0Proc\u00e9dure de pr\u00e9paration d\u2019\u00e9chantillons pour l\u2019analyse de pesticides, mycotoxines et cannabino\u00efdes dans les bonbons g\u00e9lifi\u00e9s au cannabis.<\/div>
\n
\n
\"\"<\/figure>\n<\/div>\n<\/div><\/div><\/div>\n\n\n
<\/div>\n\n\n\n

Quantification<\/h3>\n\n\n\n

Pour l\u2019analyse des pesticides et des mycotoxines, des solutions de calibration ont \u00e9t\u00e9 pr\u00e9par\u00e9es par dopage des analytes et des standards internes dans des aliquotes d\u2019extraits obtenus \u00e0 partir de blancs de bonbons g\u00e9lifi\u00e9s (la solution a \u00e9t\u00e9 obtenue en m\u00e9langeant des extraits de plusieurs blancs de bonbons g\u00e9lifi\u00e9s). Le Tableau I montre les volumes de la solution de dopage des analytes cibles et de la solution de standards internes qui ont \u00e9t\u00e9 ajout\u00e9s \u00e0 chaque aliquote (volume final de la solution de calibration = 3 mL). Pour r\u00e9aliser les courbes de calibration pour les pesticides analysables par GC, 1.9 mL des solutions de calibration de 3 mL ont \u00e9t\u00e9 soumis \u00e0 une purification par dSPE comme cela est d\u00e9crit dans la section sur la pr\u00e9paration des \u00e9chantillons. L\u2019exactitude et la pr\u00e9cision de la m\u00e9thode ont \u00e9t\u00e9 \u00e9valu\u00e9es en dopant un m\u00e9lange homog\u00e9n\u00e9is\u00e9 de bonbons g\u00e9lifi\u00e9s (apr\u00e8s addition d\u2019eau et passage au vortex) \u00e0 10, 50, 100 et 500 ng\/g en quatre r\u00e9plicas (Tableau II), et en effectuant la proc\u00e9dure compl\u00e8te de pr\u00e9paration d\u2019\u00e9chantillons d\u00e9crite dans la section sur la pr\u00e9paration des \u00e9chantillons.<\/p>\n\n\n\n

Pour l\u2019analyse des cannabino\u00efdes, les solutions de calibration ont \u00e9t\u00e9 pr\u00e9par\u00e9es \u00e0 2, 5, 10, 20, 50, 100 et 200 ppm dans une solution ac\u00e9tonitrile:eau 75:25. Les rendements pour les cannabino\u00efdes ont \u00e9t\u00e9 \u00e9valu\u00e9s en dopant les \u00e9chantillons de bonbons g\u00e9lifi\u00e9s (1 g) solubilis\u00e9s dans l\u2019eau \u00e0 0.2 et 0.5 mg\/g (n=2) puis en les extrayant comme d\u00e9crit pr\u00e9c\u00e9demment.<\/p>\n\n\n\n

Tableau I :<\/strong> Pr\u00e9paration des \u00e9talons pour l\u2019analyse des pesticides et des mycotoxines \u00e0 l\u2019aide d\u2019aliquotes extraits \u00e0 partir d\u2019\u00e9chantillons blancs de bonbons g\u00e9lifi\u00e9s (volume final de chaque solution de calibration = 3 mL).<\/p>\n\n\n\n

Conc. souhait\u00e9e de l\u2019analyte en matrice (ng\/g)<\/strong><\/td>Conc. de l\u2019analyte dans l\u2019extrait final en supposant un rendement d\u2019extraction de la matrice \u00e0 100% (ng\/mL)<\/strong><\/td>\u00b5L de solution d\u2019analyte cible ajout\u00e9s au blanc extrait<\/strong><\/td>Conc. de l\u2019analyte dans la solution de dopage (ng\/mL)<\/strong><\/td>\u00b5L du m\u00e9lange de standards internes \u00e0 5000 ng\/mL ajout\u00e9s au blanc extrait<\/strong><\/td><\/tr>
5<\/td>1<\/td>30<\/td>100<\/td>24<\/td><\/tr>
20<\/td>4<\/td>12<\/td>1000<\/td>24<\/td><\/tr>
50<\/td>10<\/td>30<\/td>1000<\/td>24<\/td><\/tr>
75<\/td>15<\/td>45<\/td>1000<\/td>24<\/td><\/tr>
150<\/td>30<\/td>90<\/td>1000<\/td>24<\/td><\/tr>
200<\/td>40<\/td>24<\/td>5000<\/td>24<\/td><\/tr>
400<\/td>80<\/td>48<\/td>5000<\/td>24<\/td><\/tr>
700<\/td>140<\/td>84<\/td>5000<\/td>24<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

Tableau II :<\/strong> Dopage en mycotoxines et pesticides dans les bonbons g\u00e9lifi\u00e9s (1 g d\u2019\u00e9chantillon homog\u00e9n\u00e9is\u00e9 avec 5 mL d\u2019eau) \u00e0 diff\u00e9rents niveaux de concentration.<\/p>\n\n\n\n

Conc. en matrice (ng\/g)<\/strong><\/td>\u00b5L de solution d\u2019analyte cible ajout\u00e9s aux \u00e9chantillons homog\u00e9n\u00e9is\u00e9s dans l\u2019eau<\/strong><\/td>Conc. de l\u2019analyte dans la solution de dopage (ng\/mL)<\/strong><\/td>\u00b5L du m\u00e9lange de standards internes \u00e0 5000 ng\/mL ajout\u00e9s aux \u00e9chantillons homog\u00e9n\u00e9is\u00e9s dans l\u2019eau<\/strong><\/td><\/tr>
10<\/td>10<\/td>1000<\/td>40<\/td><\/tr>
50<\/td>50<\/td>1000<\/td>40<\/td><\/tr>
100<\/td>100<\/td>1000<\/td>40<\/td><\/tr>
500<\/td>100<\/td>5000<\/td>40<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

Instrument Conditions<\/h3>\n\n\n\n

L\u2019instrumentation et les conditions d\u2019analyse des pesticides, mycotoxines et cannabino\u00efdes dans les bonbons g\u00e9lifi\u00e9s au cannabis sont pr\u00e9sent\u00e9es dans les Tableaux III, IV et V. Les transitions MRM des contaminants analysables par LC et des contaminants analysables par GC sont pr\u00e9sent\u00e9es respectivement dans les Tableaux VI et VII. Les temps de r\u00e9tention des cannabino\u00efdes sont pr\u00e9sent\u00e9s dans le Tableau VIII.<\/p>\n\n\n\n

Tableau III :<\/strong> Conditions LC-MS\/MS (Pesticides et Mycotoxines).<\/p>\n\n\n\n

Colonne<\/strong><\/td>Raptor ARC-18 2.7 \u00b5m, 100 mm x 2.1 mm (r\u00e9f. 9314A12)<\/td><\/tr>
Pr\u00e9colonne<\/strong><\/td>Pr\u00e9colonne EXP Raptor ARC-18, 2.1 x 5 mm, 2.7\u00b5m (r\u00e9f. 9314A0252)<\/td><\/tr>
Phase mobile A<\/strong><\/td>Eau, formiate d\u2019ammonium 2 mM, 0.1% d\u2019acide formique<\/td><\/tr>
Phase mobile B<\/strong><\/td>M\u00e9thanol, formiate d\u2019ammonium 2 mM, 0.1% d\u2019acide formique<\/td><\/tr>
Gradient<\/strong><\/td>Temps (min)<\/td>%B<\/td>Temps (min)<\/td>%B<\/td><\/tr>
0<\/td>5<\/td>10.5<\/td>100<\/td><\/tr>
1.5<\/td>65<\/td>10.6<\/td>5<\/td><\/tr>
8.5<\/td>95<\/td>12.0<\/td>5<\/td><\/tr>
9.5<\/td>100<\/td>–<\/td>–<\/td><\/tr>
D\u00e9bit<\/strong><\/td>0.5 mL\/min<\/td><\/tr>
Temp. du four \u00e0 colonne<\/strong><\/td>40 \u00b0C<\/td><\/tr>
Temp. du passeur d’\u00e9chantillons<\/strong><\/td>10 \u00b0C<\/td><\/tr>
Volume inject\u00e9<\/strong><\/td>2 \u03bcL<\/td><\/tr>
Instrument<\/strong><\/td>Shimadzu LCMS-8060<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

Tableau IV :<\/strong> Conditions GC-MS\/MS (Pesticides).<\/p>\n\n\n\n

Instrument<\/strong><\/td>Thermo Trace 1310-TSQ 8000<\/td><\/tr>
Colonne<\/strong><\/td>Rxi-5ms, 30 m x 0.25 mm DI x 0.25 \u00b5m (r\u00e9f# 13423)<\/td><\/tr>
Injection Mode<\/strong><\/td>Splitless<\/td><\/tr>
Inj. Vol.<\/strong><\/td>1 \u00b5L<\/td><\/tr>
Insert d’injection<\/strong><\/td>Topaz 4.0 mm ID \u201cSingle Taper\u201d avec laine (r\u00e9f# 23447)<\/td><\/tr>
Volume inject\u00e9<\/strong><\/td>250 \u00b0C<\/td><\/tr>
D\u00e9bit de split<\/strong><\/td>14.0 mL\/min<\/td><\/tr>
Temps splitless<\/strong><\/td>0.50 min<\/td><\/tr>
D\u00e9bit de purge<\/strong><\/td>5 mL\/min<\/td><\/tr>
Four<\/strong><\/td>90 \u00b0C (maintien pendant 1 min) \u00e0 310 \u00b0C \u00e0 25 \u00b0C\/min (maintien 10 min)<\/td><\/tr>
Gaz vecteur<\/strong><\/td>He, d\u00e9bit constant<\/td><\/tr>
D\u00e9bit<\/strong><\/td>1.40 mL\/min<\/td><\/tr>
D\u00e9tecteur<\/strong><\/td>MS\/MS<\/td><\/tr>
Type de m\u00e9thode<\/strong><\/td>Acquisition – chronom\u00e9tr\u00e9<\/td><\/tr>
Mode d’ionisation<\/strong><\/td>Impact \u00e9lectronique (EI)<\/td><\/tr>
Temp\u00e9rature de la ligne de transfert<\/strong><\/td>290 \u00b0C<\/td><\/tr>
Temp\u00e9rature de la source<\/strong><\/td>330 \u00b0C<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

Tableau V :<\/strong> Conditions HPLC-UV (pour l\u2019analyse de puissance en utilisant une m\u00e9thode d\u2019\u00e9conomie des solvants [3]).<\/p>\n\n\n\n

Instrument<\/strong><\/td>Waters ACQUITY<\/td><\/tr>
Colonne<\/strong><\/td>Raptor ARC-18, 2.1 x 150 mm, 2.7 \u00b5m (r\u00e9f# 9314A62)<\/td><\/tr>
Pr\u00e9colonne<\/strong><\/td>Pr\u00e9-colonne EXP Raptor ARC-18, 2.1 x 5 mm, 2.7\u00b5m (r\u00e9f# 9314A0252)<\/td><\/tr>
Volume inject\u00e9<\/strong><\/td>2 \u00b5L<\/td><\/tr>
Phase mobile A<\/strong><\/td>Eau, formiate d\u2019ammonium 5 mM, 0.1% d\u2019acide formique<\/td><\/tr>
Phase mobile B<\/strong><\/td>Ac\u00e9tonitrile, 0.1% d\u2019acide formique<\/td><\/tr>
Gradient<\/strong><\/td>Isocratique \u00e0 75% B<\/td><\/tr>
D\u00e9bit<\/strong><\/td>0.4 mL\/min<\/td><\/tr>
Temp. du four \u00e0 colonne<\/strong><\/td>30 \u00b0C<\/td><\/tr>
Temp. du passeur d’\u00e9chantillons<\/strong><\/td>10 \u00b0C<\/td><\/tr>
Longueur d’onde<\/strong><\/td>228 nm<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

Tableau VI :<\/strong> Transitions LC-MS\/MS<\/p>\n\n\n\n

Nom<\/strong><\/td>Temps de r\u00e9tention (min)<\/strong><\/td>Ion pr\u00e9curseur<\/strong><\/td>Ion produit 1<\/strong><\/td>Ion produit 2<\/strong><\/td><\/tr>
Daminozide-D6<\/td>0.7<\/td>167.0<\/td>149.3<\/td>49.3<\/td><\/tr>
Daminozide<\/td>0.7<\/td>161.1<\/td>44.1<\/td>143.2<\/td><\/tr>
Acephate<\/td>1.7<\/td>184.0<\/td>143.1<\/td>95.1<\/td><\/tr>
Oxamyl<\/td>2.0<\/td>237.1<\/td>72.1<\/td>90.1<\/td><\/tr>
Flonicamid<\/td>2.1<\/td>230.1<\/td>203.1<\/td>174.1<\/td><\/tr>
Methomyl<\/td>2.1<\/td>163.1<\/td>88.1<\/td>106.1<\/td><\/tr>
Thiamethoxam<\/td>2.1<\/td>292.0<\/td>211.1<\/td>181.1<\/td><\/tr>
Imidacloprid<\/td>2.3<\/td>256.1<\/td>209.1<\/td>175.1<\/td><\/tr>
Mevinphos<\/td>2.4<\/td>225.1<\/td>127.1<\/td>193.2<\/td><\/tr>
Acetamiprid<\/td>2.4<\/td>223.0<\/td>126.1<\/td>56.1<\/td><\/tr>
Dimethoathe-D6<\/td>2.4<\/td>236.1<\/td>205.1<\/td>–<\/td><\/tr>
Dimethoate<\/td>2.4<\/td>230.0<\/td>199.1<\/td>125.1<\/td><\/tr>
Thiacloprid<\/td>2.5<\/td>253.0<\/td>126.0<\/td>90.1<\/td><\/tr>
Aflatoxin G2<\/td>2.5<\/td>331.2<\/td>189.3<\/td>115.2<\/td><\/tr>
Aflatoxin G1<\/td>2.5<\/td>329.2<\/td>243.2<\/td>215.3<\/td><\/tr>
Aldicarb<\/td>2.6<\/td>116.0<\/td>89.2<\/td>70.2<\/td><\/tr>
Aflatoxin B2<\/td>2.6<\/td>315.3<\/td>287.2<\/td>243.3<\/td><\/tr>
Dichlorvos<\/td>2.7<\/td>220.9<\/td>109.1<\/td>79.2<\/td><\/tr>
Dichlorvos-D6<\/td>2.7<\/td>227.0<\/td>115.1<\/td>–<\/td><\/tr>
Aflatoxin B1<\/td>2.7<\/td>313.2<\/td>241.2<\/td>128.2<\/td><\/tr>
Imazalil<\/td>2.7<\/td>297.0<\/td>159.0<\/td>201.0<\/td><\/tr>
Carbofuran<\/td>2.7<\/td>222.1<\/td>123.1<\/td>165.2<\/td><\/tr>
Propoxur<\/td>2.7<\/td>210.1<\/td>111.1<\/td>93.1<\/td><\/tr>
Carbaryl-D7<\/td>2.8<\/td>209.2<\/td>152.2<\/td>–<\/td><\/tr>
Carbaryl<\/td>2.8<\/td>202.1<\/td>145.1<\/td>127.1<\/td><\/tr>
Diuron-D6<\/td>3.0<\/td>239.1<\/td>78.2<\/td>–<\/td><\/tr>
Atrazine-D5<\/td>3.0<\/td>221.2<\/td>179.1<\/td>–<\/td><\/tr>
Naled<\/td>3.1<\/td>397.8<\/td>127.1<\/td>109.1<\/td><\/tr>
Metalaxyl<\/td>3.1<\/td>280.2<\/td>220.2<\/td>192.2<\/td><\/tr>
Spiroxamine<\/td>3.1<\/td>298.3<\/td>144.2<\/td>100.2<\/td><\/tr>
Chlorantraniliprole<\/td>3.2<\/td>483.9<\/td>452.9<\/td>285.9<\/td><\/tr>
Phosmet<\/td>3.2<\/td>318.0<\/td>160.1<\/td>77.2<\/td><\/tr>
Azoxystrobin<\/td>3.3<\/td>404.0<\/td>372.1<\/td>344.1<\/td><\/tr>
Linuron-D6<\/td>3.3<\/td>255.1<\/td>160.1<\/td>–<\/td><\/tr>
Fludioxonil*<\/td>3.4<\/td>247.0<\/td>180.0<\/td>126.0<\/td><\/tr>
Methiocarb<\/td>3.4<\/td>226.1<\/td>169.1<\/td>121.1<\/td><\/tr>
Dimethomorph<\/td>3.5<\/td>388.2<\/td>301.2<\/td>165.3<\/td><\/tr>
Boscalid<\/td>3.5<\/td>342.9<\/td>307.1<\/td>140.1<\/td><\/tr>
Paclobutrazol<\/td>3.6<\/td>294.3<\/td>70.1<\/td>125.1<\/td><\/tr>
Malathion<\/td>3.6<\/td>331.0<\/td>127.2<\/td>285.2<\/td><\/tr>
Myclobutanil<\/td>3.7<\/td>289.1<\/td>70.1<\/td>125.1<\/td><\/tr>
Bifenazate<\/td>3.7<\/td>301.0<\/td>198.1<\/td>170.2<\/td><\/tr>
Ochratoxin A<\/td>3.8<\/td>404.2<\/td>239.1<\/td>358.3<\/td><\/tr>
Fenhexamid<\/td>3.9<\/td>302.1<\/td>97.1<\/td>55.2<\/td><\/tr>
Spirotetramat<\/td>4.0<\/td>374.2<\/td>302.1<\/td>216.1<\/td><\/tr>
Ethoprophos<\/td>4.1<\/td>243.1<\/td>131.1<\/td>97.1<\/td><\/tr>
Fipronil*<\/td>4.1<\/td>436.8<\/td>331.8<\/td>251.9<\/td><\/tr>
Fenoxycarb<\/td>4.2<\/td>302.1<\/td>88.1<\/td>116.1<\/td><\/tr>
Kresoxim methyl<\/td>4.4<\/td>314.2<\/td>267.2<\/td>222.2<\/td><\/tr>
Tebuconazole<\/td>4.4<\/td>308.1<\/td>70.1<\/td>125.1<\/td><\/tr>
Diazinon-D10<\/td>4.6<\/td>315.2<\/td>170.2<\/td>–<\/td><\/tr>
Spinosad (spinosyn A)<\/td>4.6<\/td>732.4<\/td>142.2<\/td>98.1<\/td><\/tr>
Diazinon<\/td>4.6<\/td>305.1<\/td>169.2<\/td>153.2<\/td><\/tr>
Coumaphos<\/td>4.7<\/td>363.1<\/td>227.1<\/td>307.1<\/td><\/tr>
Pyridaben<\/td>4.7<\/td>365.1<\/td>309.2<\/td>147.2<\/td><\/tr>
Propiconazole<\/td>4.7<\/td>342.0<\/td>159.0<\/td>69.2<\/td><\/tr>
Clofentezine<\/td>4.8<\/td>303.0<\/td>138.1<\/td>102.1<\/td><\/tr>
Spinosad (spinosyn D)<\/td>5.0<\/td>746.5<\/td>142.3<\/td>98.4<\/td><\/tr>
Spinetoram (spinosyn J)<\/td>5.1<\/td>748.5<\/td>142.3<\/td>98.3<\/td><\/tr>
Trifloxystrobin<\/td>5.3<\/td>409.2<\/td>186.1<\/td>145.1<\/td><\/tr>
Prallethrin<\/td>5.3<\/td>301.2<\/td>123.2<\/td>105.2<\/td><\/tr>
Pyrethrin II<\/td>5.5<\/td>373.1<\/td>161.1<\/td>133.2<\/td><\/tr>
Spinetoram (spinosyn L)<\/td>5.6<\/td>760.5<\/td>142.2<\/td>98.1<\/td><\/tr>
Piperonyl butoxide<\/td>6.0<\/td>356.3<\/td>177.2<\/td>119.2<\/td><\/tr>
Chlorpyrifos<\/td>6.1<\/td>349.9<\/td>198.0<\/td>97.1<\/td><\/tr>
Hexythiazox<\/td>6.2<\/td>353.1<\/td>228.1<\/td>168.1<\/td><\/tr>
Etoxazole<\/td>6.6<\/td>360.2<\/td>141.1<\/td>304.2<\/td><\/tr>
Spiromesifen<\/td>6.7<\/td>273.2<\/td>255.2<\/td>187.2<\/td><\/tr>
Pyrethrin I<\/td>6.9<\/td>329.2<\/td>161.2<\/td>105.2<\/td><\/tr>
Cyfluthrin (qualifier)<\/td>6.9<\/td>453.1<\/td>193.2<\/td>–<\/td><\/tr>
Cyfluthrin<\/td>6.9<\/td>451.1<\/td>191.2<\/td>–<\/td><\/tr>
Cypermethrin<\/td>7.1<\/td>433.1<\/td>191.0<\/td>416.0<\/td><\/tr>
(E)-Fenpyroximate<\/td>7.1<\/td>422.2<\/td>366.1<\/td>138.1<\/td><\/tr>
Permethrin-trans<\/em><\/td>7.6<\/td>408.3<\/td>183.2<\/td>355.1<\/td><\/tr>
Permethrin-cis<\/em><\/td>7.9<\/td>408.3<\/td>183.2<\/td>355.1<\/td><\/tr>
Avermectin B1a<\/td>7.9<\/td>890.5<\/td>305.4<\/td>567.4<\/td><\/tr>
Etofenprox<\/td>8.0<\/td>394.3<\/td>177.2<\/td>359.3<\/td><\/tr>
Bifenthrin<\/td>8.2<\/td>440.0<\/td>181.2<\/td>166.2<\/td><\/tr>
Acequinocyl precursor ion 1<\/td>9.4<\/td>402.3<\/td>343.2<\/td>189.0<\/td><\/tr>
Acequinocyl precursor ion 2<\/td>9.4<\/td>386.0<\/td>344.2<\/td>189.1<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

*Analyses r\u00e9alis\u00e9es en mode n\u00e9gatif.<\/p>\n\n\n\n

Tableau VII :<\/strong> transitions GC-MS\/MS.<\/p>\n\n\n\n

Nom<\/strong><\/td>Temps de r\u00e9tention (min)<\/strong><\/td>Polarit\u00e9<\/strong><\/td>Ion pr\u00e9curseur<\/strong><\/td>Ion produit<\/strong><\/td><\/tr>
Atrazine-D5 (IS) (Quan)<\/td>6.82<\/td>Positive<\/td>220.0<\/td>58.0<\/td><\/tr>
Atrazine-D5 (IS) (Qual)<\/td>6.82<\/td>Positive<\/td>205.0<\/td>127.0<\/td><\/tr>
Diazinon-D10 (Quan)<\/td>7.01<\/td>Positive<\/td>183.0<\/td>139.0<\/td><\/tr>
Diazinon-D10 (Qual)<\/td>7.01<\/td>Positive<\/td>183.0<\/td>168.0<\/td><\/tr>
Quintozene (PCNB) (Quan)<\/td>7.03<\/td>Positive<\/td>294.9<\/td>236.9<\/td><\/tr>
Quintozene (PCNB) (Qual)<\/td>7.03<\/td>Positive<\/td>236.8<\/td>118.9<\/td><\/tr>
Methyl parathion (Quan)<\/td>7.50<\/td>Positive<\/td>263.0<\/td>109.0<\/td><\/tr>
Methyl parathion (Qual)<\/td>7.50<\/td>Positive<\/td>263.0<\/td>79.0<\/td><\/tr>
Captan (Quan)<\/td>8.37<\/td>Positive<\/td>184.0<\/td>149.1<\/td><\/tr>
Captan (Qual)<\/td>8.37<\/td>Positive<\/td>184.0<\/td>134.1<\/td><\/tr>
trans<\/em>-Chlordane (Quan)<\/td>8.41<\/td>Positive<\/td>271.9<\/td>237.0<\/td><\/tr>
trans<\/em>-Chlordane (Qual)<\/td>8.41<\/td>Positive<\/td>372.9<\/td>265.9<\/td><\/tr>
cis<\/em>-Chlordane (Quan)<\/td>8.53<\/td>Positive<\/td>372.9<\/td>265.9<\/td><\/tr>
cis<\/em>-Chlordane (Qual)<\/td>8.53<\/td>Positive<\/td>271.9<\/td>237.0<\/td><\/tr>
Chlorfenapyr (Quan)<\/td>8.80<\/td>Positive<\/td>247.1<\/td>227.1<\/td><\/tr>
Chlorfenapyr (Qual)<\/td>8.80<\/td>Positive<\/td>59.1<\/td>31.1<\/td><\/tr>
Cyfluthrin (Quan)<\/td>10.61<\/td>Positive<\/td>226.0<\/td>206.0<\/td><\/tr>
Cyfluthrin (Qual)<\/td>10.61<\/td>Positive<\/td>163.0<\/td>127.0<\/td><\/tr>
Cypermethrin (Quan)<\/td>10.87<\/td>Positive<\/td>163.0<\/td>127.1<\/td><\/tr>
Cypermethrin (Qual)<\/td>10.87<\/td>Positive<\/td>181.1<\/td>152.1<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

Table VIII:<\/strong> Cannabinoid Retention Times.<\/p>\n\n\n\n

Compound<\/strong><\/td>Retention Time (min)<\/strong><\/td><\/tr>
Cannabidiolic acid (CBDA)<\/td>2.142<\/td><\/tr>
Cannabigerol (CBG)<\/td>2.405<\/td><\/tr>
Cannabidiol (CBD)<\/td>2.535<\/td><\/tr>
Cannabinol (CBN)<\/td>3.776<\/td><\/tr>
Delta-9-tetrahydrocannabinol (Delta-9-THC)<\/td>4.753<\/td><\/tr>
Tetrahydrocannabinolic acid (THCA)<\/td>6.279<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n
<\/div>\n\n\n\n

R\u00e9sultats et interpr\u00e9tation<\/h2>\n\n\n\n

Optimisation de la m\u00e9thode<\/h3>\n\n\n\n

Vu la diversit\u00e9 des matrices d\u00e9riv\u00e9es du cannabis et les diff\u00e9rences dans les caract\u00e9ristiques chimiques des analytes cibles, de nombreuses strat\u00e9gies existent pour garantir des r\u00e9sultats pr\u00e9cis. L’analyse des pesticides, des mycotoxines et des cannabino\u00efdes dans les bonbons g\u00e9lifi\u00e9s au cannabis, comme l’exige l’\u00c9tat de Californie, n\u00e9cessitait des conditions exp\u00e9rimentales compl\u00e8tement diff\u00e9rentes de celles utilis\u00e9es dans notre article technique pr\u00e9c\u00e9dent pour l\u2019analyse dans les brownies [4]. Tout d’abord, nous avons observ\u00e9 que l\u2019utilisation des bonbons g\u00e9lifi\u00e9s \u00ab pulv\u00e9ris\u00e9s \u00bb (le broyage a \u00e9t\u00e9 effectu\u00e9 \u00e0 l’aide de neige carbonique et d’un robot culinaire) peut se r\u00e9v\u00e9ler extr\u00eamement difficile car la matrice devient extr\u00eamement collante une fois revenue \u00e0 temp\u00e9rature ambiante. Pour cette raison, couper les bonbons g\u00e9lifi\u00e9s en petits morceaux s’est av\u00e9r\u00e9 \u00eatre une bien meilleure alternative, qui a facilit\u00e9 la pes\u00e9e exacte de l\u2019\u00e9chantillon.<\/p>\n\n\n\n

Le d\u00e9fi suivant a consist\u00e9 \u00e0 trouver la meilleure approche pour dissoudre la matrice avant son extraction afin d’obtenir des donn\u00e9es fiables. Comme l’\u00e9chantillon \u00e9tait d\u00e9coup\u00e9 en petits morceaux de taille al\u00e9atoire, avoir une matrice homog\u00e8ne \u00e9tait crucial pour garantir une reproductibilit\u00e9 satisfaisante de la m\u00e9thode. Tout d’abord, nous avons \u00e9valu\u00e9 l’utilisation de solvants tels que l’ac\u00e9tonitrile et le m\u00e9thanol pour dissoudre les morceaux de bonbons g\u00e9lifi\u00e9s, et pour extraire les analytes d’int\u00e9r\u00eat (comme une simple extraction par solvant). Cependant, nous avons constat\u00e9 qu’il \u00e9tait tr\u00e8s difficile de solubiliser la matrice dans ces conditions. Nous avons \u00e9galement \u00e9valu\u00e9 l’utilisation du DMSO \u00e0 cette fin. M\u00eame si tous les morceaux de bonbons g\u00e9lifi\u00e9s ont \u00e9t\u00e9 facilement dissous dans ce solvant, le daminozide n’a \u00e9t\u00e9 d\u00e9tect\u00e9 dans aucun des extraits en raison de la suppression ionique due au faible pourcentage de DMSO restant dans les \u00e9chantillons inject\u00e9s. Apr\u00e8s ces tests, nous avons conclu que l’hydratation de l’\u00e9chantillon avec 5 ml d’eau suivie d’un m\u00e9lange vigoureux au vortex \u00e9tait le meilleur moyen d’obtenir un \u00e9chantillon homog\u00e8ne. Par la suite, pour extraire tous les contaminants de la matrice, 5 ml d’ac\u00e9tonitrile acidifi\u00e9 \u00e0 1 % avec de l’acide ac\u00e9tique ont \u00e9t\u00e9 ajout\u00e9s \u00e0 l’\u00e9chantillon dissous.<\/p>\n\n\n\n

Pour s\u00e9parer la phase organique de la phase, trois sels d’extraction QuEChERS Q-sep diff\u00e9rents ont \u00e9t\u00e9 compar\u00e9s : AOAC (r\u00e9f. 25851), non tamponn\u00e9 (r\u00e9f. 25847), et EN (r\u00e9f. 25849). ELes sels EN ont donn\u00e9 les meilleurs r\u00e9sultats, avec tous les compos\u00e9s ayant des rendements sup\u00e9rieurs \u00e0 83 %, \u00e0 l’exception du daminozide et de son analogue deut\u00e9r\u00e9, qui ont montr\u00e9 des rendements d’environ 25 %. Pour l’\u00e9tape de nettoyage\/purification, quatre m\u00e9langes diff\u00e9rents de sorbants QuEChERS dSPE Q-sep (r\u00e9f.\u00a026215,\u00a026216,\u00a026217,\u00a026242) ont \u00e9t\u00e9 \u00e9valu\u00e9s pour tous les pesticides analysables par LC-MS. Il a \u00e9t\u00e9 confirm\u00e9 que tous les m\u00e9langes contenant 25 mg de PSA (r\u00e9f.\u00a026215,\u00a026216,\u00a026217) entra\u00eenaient des pertes importantes de daminozide et d’ochratoxine A avec des rendements de l\u2019ordre de 40 %. Le m\u00e9lange dSPE contenant du MgSO4 et du C18 (r\u00e9f. 26242) n’a pas entra\u00een\u00e9 de pertes significatives de pesticides ; malgr\u00e9 tout, nous avons d\u00e9cid\u00e9 d’\u00e9valuer la pertinence d’utiliser l’extrait organique sans aucune autre \u00e9tape de nettoyage\/purification pour la quantification des compos\u00e9s analysables par LC.<\/p>\n\n\n\n

Pour \u00e9valuer la faisabilit\u00e9 de l’analyse directe des extraits, des exp\u00e9riences visant \u00e0 \u00e9tudier les effets matrice dans les extraits de bonbons g\u00e9lifi\u00e9s sans aucune \u00e9tape de nettoyage\/purification ont \u00e9t\u00e9 men\u00e9es en utilisant la m\u00e9thodologie propos\u00e9e par Matuszweski et al. [5]. Les extraits obtenus \u00e0 partir d’\u00e9chantillons “blancs” ont \u00e9t\u00e9 dop\u00e9s \u00e0 des concentrations finales de 5, 15 et 50 ppb, et leurs r\u00e9ponses ont \u00e9t\u00e9 compar\u00e9es au solvant pur dop\u00e9 avec les m\u00eames niveaux de concentration \u00e0 l\u2019aide d\u2019une analyse LC-MS\/MS. \u00c0 5 ppb, 12 pesticides ont montr\u00e9 des effets matrice sup\u00e9rieurs \u00e0 120 %, et \u00e0 15 ppb et 50 ppb, seul le daminozide a montr\u00e9 un gain significatif (Tableau IX). De par ces informations et \u00e0 cause du faible rendement obtenu pour le daminozide, l’utilisation du daminozide-d6 comme \u00e9talon interne a donc \u00e9t\u00e9 cruciale pour obtenir des donn\u00e9es fiables.<\/p>\n\n\n\n

Concernant les rendements des pesticides analysables par GC, les donn\u00e9es correspondant \u00e0 l’\u00e9valuation de trois m\u00e9langes de sorbants dSPE (r\u00e9f.\u00a026215,\u00a026216, et\u00a026217) ont montr\u00e9 que, dans tous les cas, les rendements \u00e9taient sup\u00e9rieurs \u00e0 96 % lorsque l’on compare la r\u00e9ponse de l’extrait purifi\u00e9 par rapport \u00e0 la r\u00e9ponse de l’extrait d’origine. Compte tenu de la teneur \u00e9lev\u00e9e en sucre et en pigments des extraits de bonbons g\u00e9lifi\u00e9s, le sorbant dSPE contenant du PSA, du GCB et du sulfate de magn\u00e9sium (r\u00e9f. 26217) a \u00e9t\u00e9 choisi pour le protocole final de pr\u00e9paration des \u00e9chantillons.<\/p>\n\n\n\n

V\u00e9rification de la m\u00e9thode<\/h3>\n\n\n\n

Le Tableau X pr\u00e9sente les r\u00e9sultats correspondant aux limites de quantification, \u00e0 la lin\u00e9arit\u00e9, \u00e0 l’exactitude et \u00e0 la pr\u00e9cision pour la liste californienne des pesticides et des mycotoxines d\u00e9termin\u00e9es dans une matrice gommeuse. Pour tous les contaminants analys\u00e9s par LC-MS\/MS, des courbes de calibration ont \u00e9t\u00e9 trac\u00e9es en utilisant des rapports de r\u00e9ponses analyte\/\u00e9talon interne et un facteur de pond\u00e9ration de 1\/x. Pour les compos\u00e9s analysables par GC, seule la courbe de calibration du PCNB a \u00e9t\u00e9 trac\u00e9e en utilisant le rapport analyte\/\u00e9talon interne, le diazinon-d10 \u00e9tant choisi comme \u00e9talon interne. Pour le reste des compos\u00e9s analysables par GC, la quantification a \u00e9t\u00e9 effectu\u00e9e avec des courbes de calibration externes (aire\/surface par rapport \u00e0 la concentration dop\u00e9e) car cela a fourni de meilleurs r\u00e9sultats qu\u2019avec l’\u00e9talon interne. Des valeurs de RSD inf\u00e9rieures \u00e0 24 % ont \u00e9t\u00e9 obtenues pour tous les analytes \u00e0 tous les niveaux de concentration test\u00e9s. Les valeurs de pr\u00e9cision \u00e9taient comprises entre 75 et 118 % et les coefficients de d\u00e9termination (R\u00b2) \u00e9taient tous sup\u00e9rieurs \u00e0 0,99.<\/p>\n\n\n\n

Enfin, les r\u00e9sultats de l’analyse des cannabino\u00efdes ont d\u00e9montr\u00e9 que l’extrait collect\u00e9 pour la d\u00e9termination des contaminants convient \u00e9galement aux analyses de puissance. Le Tableau XI pr\u00e9sente les donn\u00e9es correspondant aux courbes de calibration pr\u00e9par\u00e9es en solvant et qui ont \u00e9t\u00e9 utilis\u00e9es pour la quantification de chaque cannabino\u00efde. Comme le montre le Tableau XII, les \u00e9chantillons de bonbons g\u00e9lifi\u00e9s dop\u00e9s avec six cannabino\u00efdes \u00e0 0,2 mg\/g ont pr\u00e9sent\u00e9 des rendements allant de 99 \u00e0 107 %, tandis que les \u00e9chantillons dop\u00e9s \u00e0 0,5 mg\/g ont montr\u00e9 des rendements de 99 \u00e0 106 %. Des chromatogrammes repr\u00e9sentatifs sont pr\u00e9sent\u00e9s dans les Figures 2 \u00e0 4.<\/p>\n\n\n\n

Tableau IX :<\/strong> Effets Matrice (EM) pour les pesticides et les mycotoxines dans les bonbons g\u00e9lifi\u00e9s au cannabis.<\/p>\n\n\n\n

 <\/td>EM \u00e0 5 ppb (%)<\/strong><\/td>RSD<\/strong><\/td>EM \u00e0 15 ppb (%)<\/strong><\/td>RSD<\/strong><\/td>EM \u00e0 50 ppb (%)<\/strong><\/td>RSD<\/strong><\/td><\/tr>
Daminozide<\/td>216<\/td>3<\/td>251<\/td>7<\/td>185<\/td>3<\/td><\/tr>
Acephate<\/td>95<\/td>6<\/td>85<\/td>1<\/td>89<\/td>6<\/td><\/tr>
Oxamyl<\/td>105<\/td>5<\/td>96<\/td>2<\/td>98<\/td>5<\/td><\/tr>
Flonicamid<\/td>91<\/td>32<\/td>90<\/td>22<\/td>97<\/td>17<\/td><\/tr>
Methomyl<\/td>104<\/td>4<\/td>92<\/td>3<\/td>99<\/td>4<\/td><\/tr>
Thiamethoxam<\/td>105<\/td>5<\/td>92<\/td>5<\/td>96<\/td>5<\/td><\/tr>
Imidacloprid<\/td>114<\/td>9<\/td>87<\/td>9<\/td>100<\/td>9<\/td><\/tr>
Mevinphos<\/td>102<\/td>6<\/td>93<\/td>3<\/td>93<\/td>6<\/td><\/tr>
Acetamiprid<\/td>100<\/td>2<\/td>88<\/td>0<\/td>91<\/td>2<\/td><\/tr>
Dimethoate<\/td>97<\/td>3<\/td>92<\/td>3<\/td>93<\/td>3<\/td><\/tr>
Thiacloprid<\/td>109<\/td>7<\/td>93<\/td>1<\/td>93<\/td>7<\/td><\/tr>
Aflatoxin G2<\/td>102<\/td>6<\/td>86<\/td>0<\/td>93<\/td>6<\/td><\/tr>
Aflatoxin G1<\/td>106<\/td>7<\/td>93<\/td>1<\/td>91<\/td>7<\/td><\/tr>
Aldicarb<\/td>81<\/td>22<\/td>85<\/td>14<\/td>90<\/td>22<\/td><\/tr>
Aflatoxin B2<\/td>113<\/td>11<\/td>79<\/td>9<\/td>95<\/td>11<\/td><\/tr>
Dichlorvos<\/td>126<\/td>15<\/td>90<\/td>6<\/td>92<\/td>15<\/td><\/tr>
Aflatoxin B1<\/td>104<\/td>9<\/td>93<\/td>5<\/td>95<\/td>9<\/td><\/tr>
Imazalil<\/td>92<\/td>1<\/td>96<\/td>3<\/td>98<\/td>1<\/td><\/tr>
Carbofuran<\/td>106<\/td>3<\/td>98<\/td>1<\/td>102<\/td>3<\/td><\/tr>
Propoxur<\/td>104<\/td>3<\/td>96<\/td>4<\/td>96<\/td>3<\/td><\/tr>
Carbaryl<\/td>103<\/td>4<\/td>99<\/td>8<\/td>93<\/td>4<\/td><\/tr>
Naled<\/td>101<\/td>4<\/td>94<\/td>2<\/td>84<\/td>4<\/td><\/tr>
Metalaxyl<\/td>105<\/td>3<\/td>97<\/td>2<\/td>97<\/td>3<\/td><\/tr>
Spiroxamine<\/td>105<\/td>4<\/td>94<\/td>1<\/td>97<\/td>4<\/td><\/tr>
Chlorantraniliprole<\/td>114<\/td>6<\/td>88<\/td>5<\/td>100<\/td>6<\/td><\/tr>
Phosmet<\/td>108<\/td>10<\/td>100<\/td>6<\/td>92<\/td>10<\/td><\/tr>
Azoxystrobin<\/td>104<\/td>1<\/td>94<\/td>1<\/td>94<\/td>1<\/td><\/tr>
Fludioxonil<\/td>101<\/td>7<\/td>90<\/td>11<\/td>94<\/td>7<\/td><\/tr>
Methiocarb<\/td>102<\/td>5<\/td>94<\/td>3<\/td>95<\/td>5<\/td><\/tr>
Dimethomorph<\/td>108<\/td>15<\/td>93<\/td>0<\/td>93<\/td>15<\/td><\/tr>
Boscalid<\/td>119<\/td>11<\/td>94<\/td>4<\/td>85<\/td>11<\/td><\/tr>
Paclobutrazol<\/td>110<\/td>10<\/td>90<\/td>2<\/td>92<\/td>10<\/td><\/tr>
Malathion<\/td>101<\/td>3<\/td>92<\/td>4<\/td>95<\/td>3<\/td><\/tr>
Myclobutanil<\/td>92<\/td>11<\/td>93<\/td>0<\/td>95<\/td>11<\/td><\/tr>
Bifenazate<\/td>105<\/td>2<\/td>98<\/td>4<\/td>99<\/td>2<\/td><\/tr>
Ochratoxin A<\/td>111<\/td>10<\/td>111<\/td>0<\/td>98<\/td>10<\/td><\/tr>
Fenhexamid<\/td>135<\/td>6<\/td>102<\/td>0<\/td>91<\/td>6<\/td><\/tr>
Spirotetramat<\/td>107<\/td>7<\/td>87<\/td>5<\/td>95<\/td>7<\/td><\/tr>
Ethoprophos<\/td>104<\/td>5<\/td>97<\/td>2<\/td>96<\/td>5<\/td><\/tr>
Fipronil<\/td>99<\/td>12<\/td>93<\/td>9<\/td>96<\/td>12<\/td><\/tr>
Fenoxycarb<\/td>108<\/td>9<\/td>97<\/td>1<\/td>93<\/td>9<\/td><\/tr>
Kresoxim methyl<\/td>93<\/td>21<\/td>108<\/td>3<\/td>90<\/td>21<\/td><\/tr>
Tebuconazole<\/td>102<\/td>6<\/td>95<\/td>3<\/td>97<\/td>6<\/td><\/tr>
Spinosyn A<\/td>100<\/td>5<\/td>98<\/td>2<\/td>95<\/td>5<\/td><\/tr>
Diazinon<\/td>107<\/td>2<\/td>95<\/td>1<\/td>96<\/td>2<\/td><\/tr>
Coumaphos<\/td>114<\/td>7<\/td>94<\/td>3<\/td>97<\/td>7<\/td><\/tr>
Pyridaben<\/td>139<\/td>18<\/td>103<\/td>15<\/td>94<\/td>18<\/td><\/tr>
Propiconazole<\/td>106<\/td>2<\/td>97<\/td>1<\/td>95<\/td>2<\/td><\/tr>
Clofentezine<\/td>126<\/td>14<\/td>87<\/td>3<\/td>92<\/td>14<\/td><\/tr>
Spinosyn D<\/td>104<\/td>8<\/td>93<\/td>8<\/td>97<\/td>8<\/td><\/tr>
Spinosyn J<\/td>110<\/td>6<\/td>92<\/td>6<\/td>101<\/td>6<\/td><\/tr>
Trifloxystrobin<\/td>103<\/td>2<\/td>95<\/td>2<\/td>101<\/td>2<\/td><\/tr>
Prallethrin<\/td>101<\/td>17<\/td>103<\/td>0<\/td>98<\/td>17<\/td><\/tr>
Pyrethrin II<\/td>92<\/td>23<\/td>82<\/td>5<\/td>101<\/td>23<\/td><\/tr>
Spinosyn L<\/td>106<\/td>6<\/td>95<\/td>0<\/td>98<\/td>6<\/td><\/tr>
Piperonyl butoxide<\/td>103<\/td>2<\/td>97<\/td>0<\/td>96<\/td>2<\/td><\/tr>
Chlorpyrifos<\/td>105<\/td>10<\/td>93<\/td>0<\/td>91<\/td>10<\/td><\/tr>
Hexythiazox<\/td>121<\/td>15<\/td>96<\/td>0<\/td>86<\/td>15<\/td><\/tr>
Etoxazole<\/td>102<\/td>1<\/td>95<\/td>1<\/td>95<\/td>1<\/td><\/tr>
Spiromesifen<\/td>112<\/td>6<\/td>95<\/td>5<\/td>100<\/td>6<\/td><\/tr>
Pyrethrin I<\/td>131<\/td>13<\/td>97<\/td>4<\/td>95<\/td>13<\/td><\/tr>
Cyfluthrin<\/td>–<\/td>–<\/td>–<\/td>–<\/td>80<\/td>8<\/td><\/tr>
Cypermethrin<\/td>–<\/td>–<\/td>95<\/td>16<\/td>96<\/td>16<\/td><\/tr>
(E)-Fenpyroximate<\/td>107<\/td>6<\/td>95<\/td>4<\/td>94<\/td>6<\/td><\/tr>
Permethrin-trans<\/em><\/td>136<\/td>22<\/td>103<\/td>4<\/td>94<\/td>22<\/td><\/tr>
Permethrin-cis<\/em><\/td>113<\/td>12<\/td>98<\/td>8<\/td>101<\/td>12<\/td><\/tr>
Avermectin B1a<\/td>122<\/td>17<\/td>96<\/td>0<\/td>87<\/td>17<\/td><\/tr>
Etofenprox<\/td>110<\/td>4<\/td>100<\/td>2<\/td>101<\/td>4<\/td><\/tr>
Bifenthrin<\/td>135<\/td>5<\/td>98<\/td>6<\/td>85<\/td>5<\/td><\/tr>
Acequinocyl<\/td>129<\/td>5<\/td>95<\/td>5<\/td>78<\/td>5<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

Tableau X :<\/strong> LQ, lin\u00e9arit\u00e9, exactitude et pr\u00e9cision pour les pesticides et mycotoxines dans les bonbons g\u00e9lifi\u00e9s au cannabis.<\/p>\n\n\n\n

Contaminant<\/strong><\/td>Niveau d\u2019action (ng\/g)<\/strong><\/td>LOQ (ng\/g)<\/strong><\/td>R2<\/sup><\/strong><\/td>10 ng\/g (n=4)<\/strong><\/td>50 ng\/g (n=4)<\/strong><\/td>100 ng\/g (n=4)<\/strong><\/td>500 ng\/g (n=4)<\/strong><\/td><\/tr>
Exactitude (%)<\/strong><\/td>Pr\u00e9cision (RSD)<\/strong><\/td>Exactitude (%)<\/strong><\/td>Pr\u00e9cision (RSD)<\/strong><\/td>Exactitude (%)<\/strong><\/td>Pr\u00e9cision (RSD)<\/strong><\/td>Exactitude (%)<\/strong><\/td>Pr\u00e9cision (RSD)<\/strong><\/td><\/tr>
Daminozide*<\/td><LOD<\/td>20<\/td>0.9999<\/td>–<\/td>–<\/td>114<\/td>6<\/td>114<\/td>4<\/td>116<\/td>4<\/td><\/tr>
Acephate<\/td>5000<\/td>5<\/td>0.9996<\/td>100<\/td>4<\/td>93<\/td>3<\/td>90<\/td>2<\/td>88<\/td>2<\/td><\/tr>
Oxamyl<\/td>200<\/td>5<\/td>0.999<\/td>108<\/td>1<\/td>102<\/td>3<\/td>105<\/td>4<\/td>99<\/td>3<\/td><\/tr>
Flonicamid<\/td>2000<\/td>50<\/td>0.999<\/td>–<\/td>–<\/td>117<\/td>6<\/td>105<\/td>11<\/td>101<\/td>4<\/td><\/tr>
Methomyl<\/td>100<\/td>20<\/td>0.9989<\/td>–<\/td>–<\/td>102<\/td>3<\/td>103<\/td>3<\/td>100<\/td>1<\/td><\/tr>
Thiamethoxam<\/td>4500<\/td>10<\/td>0.9988<\/td>112<\/td>23<\/td>108<\/td>5<\/td>108<\/td>6<\/td>100<\/td>3<\/td><\/tr>
Imidacloprid<\/td>3000<\/td>10<\/td>0.9985<\/td>105<\/td>17<\/td>107<\/td>3<\/td>109<\/td>4<\/td>102<\/td>5<\/td><\/tr>
Mevinphos (I and II)*<\/td><LOD<\/td>20<\/td>0.9981<\/td>–<\/td>–<\/td>101<\/td>4<\/td>104<\/td>7<\/td>101<\/td>3<\/td><\/tr>
Acetamiprid<\/td>5000<\/td>10<\/td>0.9968<\/td>100<\/td>8<\/td>108<\/td>6<\/td>109<\/td>5<\/td>105<\/td>1<\/td><\/tr>
Dimethoate*<\/td><LOD<\/td>5<\/td>0.9994<\/td>109<\/td>15<\/td>104<\/td>3<\/td>101<\/td>5<\/td>99<\/td>2<\/td><\/tr>
Thiacloprid*<\/td><LOD<\/td>20<\/td>0.9981<\/td>–<\/td>–<\/td>100<\/td>1<\/td>103<\/td>4<\/td>103<\/td>3<\/td><\/tr>
Aflatoxin G2<\/td>20#<\/sup><\/td>5<\/td>0.9957<\/td>112<\/td>17<\/td>101<\/td>6<\/td>97<\/td>2<\/td>–<\/td>–<\/td><\/tr>
Aflatoxin G1<\/td>20#<\/sup><\/td>5<\/td>0.9984<\/td>114<\/td>9<\/td>98<\/td>1<\/td>100<\/td>4<\/td>–<\/td>–<\/td><\/tr>
Aldicarb*<\/td><LOD<\/td>20<\/td>0.9971<\/td>–<\/td>–<\/td>91<\/td>17<\/td>104<\/td>8<\/td>97<\/td>4<\/td><\/tr>
Aflatoxin B2<\/td>20#<\/sup><\/td>5<\/td>0.9973<\/td>97<\/td>23<\/td>107<\/td>6<\/td>94<\/td>7<\/td>–<\/td>–<\/td><\/tr>
Dichlorvos*<\/td><LOD<\/td>10<\/td>0.9984<\/td>98<\/td>17<\/td>103<\/td>4<\/td>97<\/td>18<\/td>106<\/td>4<\/td><\/tr>
Aflatoxin B1<\/td>20#<\/sup><\/td>5<\/td>0.9978<\/td>113<\/td>5<\/td>101<\/td>6<\/td>96<\/td>5<\/td>–<\/td>–<\/td><\/tr>
Imazalil*<\/td><LOD<\/td>5<\/td>0.9977<\/td>97<\/td>19<\/td>109<\/td>5<\/td>107<\/td>4<\/td>105<\/td>3<\/td><\/tr>
Carbofuran*<\/td><LOD<\/td>5<\/td>0.9973<\/td>93<\/td>7<\/td>108<\/td>1<\/td>109<\/td>5<\/td>99<\/td>4<\/td><\/tr>
Propoxur*<\/td><LOD<\/td>5<\/td>0.9977<\/td>108<\/td>6<\/td>108<\/td>2<\/td>107<\/td>4<\/td>102<\/td>3<\/td><\/tr>
Carbaryl<\/td>500<\/td>5<\/td>0.9988<\/td>95<\/td>14<\/td>109<\/td>6<\/td>108<\/td>5<\/td>102<\/td>2<\/td><\/tr>
Naled<\/td>500<\/td>5<\/td>0.9968<\/td>98<\/td>4<\/td>112<\/td>8<\/td>110<\/td>3<\/td>101<\/td>5<\/td><\/tr>
Metalaxyl<\/td>15,000<\/td>5<\/td>0.9988<\/td>101<\/td>5<\/td>105<\/td>4<\/td>106<\/td>5<\/td>99<\/td>3<\/td><\/tr>
Spiroxamine*<\/td><LOD<\/td>5<\/td>0.9977<\/td>104<\/td>6<\/td>106<\/td>2<\/td>105<\/td>2<\/td>101<\/td>3<\/td><\/tr>
Chlorantraniliprole<\/td>40,000<\/td>20<\/td>0.9971<\/td>–<\/td>–<\/td>93<\/td>7<\/td>104<\/td>6<\/td>104<\/td>5<\/td><\/tr>
Phosmet<\/td>200<\/td>5<\/td>0.9992<\/td>109<\/td>14<\/td>105<\/td>3<\/td>104<\/td>3<\/td>100<\/td>4<\/td><\/tr>
Azoxystrobin<\/td>40,000<\/td>5<\/td>0.9992<\/td>100<\/td>3<\/td>104<\/td>1<\/td>105<\/td>4<\/td>102<\/td>3<\/td><\/tr>
Fludioxonil<\/td>30,000<\/td>20<\/td>0.9949<\/td>–<\/td>–<\/td>109<\/td>13<\/td>97<\/td>6<\/td>101<\/td>6<\/td><\/tr>
Methiocarb*<\/td><LOD<\/td>5<\/td>0.9988<\/td>116<\/td>16<\/td>105<\/td>5<\/td>107<\/td>5<\/td>101<\/td>4<\/td><\/tr>
Dimethomorph (I and II)<\/td>20,000<\/td>10<\/td>0.999<\/td>75<\/td>14<\/td>101<\/td>6<\/td>93<\/td>8<\/td>101<\/td>5<\/td><\/tr>
Boscalid<\/td>10,000<\/td>10<\/td>0.9964<\/td>108<\/td>15<\/td>102<\/td>12<\/td>102<\/td>2<\/td>103<\/td>3<\/td><\/tr>
Paclobutrazol*<\/td><LOD<\/td>10<\/td>0.9979<\/td>99<\/td>9<\/td>106<\/td>1<\/td>108<\/td>3<\/td>100<\/td>4<\/td><\/tr>
Malathion<\/td>5000<\/td>10<\/td>0.9989<\/td>117<\/td>12<\/td>112<\/td>3<\/td>106<\/td>2<\/td>101<\/td>3<\/td><\/tr>
Myclobutanil<\/td>9000<\/td>10<\/td>0.9986<\/td>102<\/td>22<\/td>102<\/td>6<\/td>104<\/td>3<\/td>101<\/td>3<\/td><\/tr>
Bifenazate<\/td>5000<\/td>10<\/td>0.9994<\/td>118<\/td>20<\/td>110<\/td>3<\/td>104<\/td>10<\/td>102<\/td>5<\/td><\/tr>
Ochratoxin A<\/td>20<\/td>10<\/td>0.9957<\/td>99<\/td>8<\/td>99<\/td>24<\/td>104<\/td>8<\/td>–<\/td>–<\/td><\/tr>
Fenhexamid<\/td>10,000<\/td>10<\/td>0.9969<\/td>96<\/td>21<\/td>109<\/td>4<\/td>106<\/td>3<\/td>107<\/td>5<\/td><\/tr>
Spirotetramat<\/td>13,000<\/td>10<\/td>0.9987<\/td>83<\/td>18<\/td>107<\/td>6<\/td>106<\/td>3<\/td>105<\/td>3<\/td><\/tr>
Ethoprophos*<\/td><LOD<\/td>5<\/td>0.9985<\/td>101<\/td>3<\/td>106<\/td>4<\/td>104<\/td>1<\/td>102<\/td>3<\/td><\/tr>
Fipronil*<\/td><LOD<\/td>20<\/td>0.998<\/td>–<\/td>–<\/td>96<\/td>5<\/td>104<\/td>8<\/td>103<\/td>4<\/td><\/tr>
Fenoxycarb*<\/td><LOD<\/td>10<\/td>0.9967<\/td>115<\/td>5<\/td>106<\/td>4<\/td>107<\/td>2<\/td>102<\/td>3<\/td><\/tr>
Kresoxym-methyl<\/td>1000<\/td>10<\/td>0.9993<\/td>112<\/td>20<\/td>104<\/td>10<\/td>102<\/td>4<\/td>103<\/td>3<\/td><\/tr>
Tebuconazole<\/td>2000<\/td>5<\/td>0.999<\/td>100<\/td>3<\/td>110<\/td>1<\/td>105<\/td>3<\/td>101<\/td>4<\/td><\/tr>
Spinosad- spinosyn A (71 %)a<\/sup><\/td>3000\u00a5<\/sup><\/td>7.1<\/td>0.9988<\/td>117<\/td>2<\/td>110<\/td>3<\/td>108<\/td>2<\/td>102<\/td>1<\/td><\/tr>
Diazinon<\/td>200<\/td>5<\/td>0.9997<\/td>104<\/td>1<\/td>102<\/td>1<\/td>104<\/td>2<\/td>101<\/td>1<\/td><\/tr>
Coumaphos*<\/td><LOD<\/td>10<\/td>0.9991<\/td>107<\/td>11<\/td>109<\/td>5<\/td>108<\/td>2<\/td>103<\/td>2<\/td><\/tr>
Pyridaben<\/td>3000<\/td>50<\/td>0.9994<\/td>–<\/td>–<\/td>93<\/td>12<\/td>113<\/td>6<\/td>103<\/td>1<\/td><\/tr>
Propiconazole<\/td>20,000<\/td>5<\/td>0.9991<\/td>96<\/td>6<\/td>108<\/td>4<\/td>104<\/td>5<\/td>103<\/td>3<\/td><\/tr>
Clofentezine<\/td>500<\/td>20<\/td>0.9978<\/td>–<\/td>–<\/td>102<\/td>5<\/td>105<\/td>3<\/td>106<\/td>4<\/td><\/tr>
Spinosad – spinosyn D (29%)b<\/sup><\/td>3000\u00a5<\/sup><\/td>2.9<\/td>0.9993<\/td>106<\/td>8<\/td>101<\/td>2<\/td>103<\/td>5<\/td>104<\/td>4<\/td><\/tr>
Spinetoram – spinosyn J (80%)c<\/sup><\/td>3000\u00a7<\/sup><\/td>4<\/td>0.9995<\/td>104<\/td>7<\/td>102<\/td>3<\/td>108<\/td>4<\/td>102<\/td>2<\/td><\/tr>
Trifloxystrobin<\/td>30,000<\/td>5<\/td>0.9996<\/td>107<\/td>3<\/td>106<\/td>3<\/td>106<\/td>3<\/td>104<\/td>2<\/td><\/tr>
Prallethrin<\/td>400<\/td>10<\/td>0.9967<\/td>107<\/td>21<\/td>99<\/td>16<\/td>111<\/td>6<\/td>101<\/td>3<\/td><\/tr>
Pyrethrin II (34%)f<\/sup><\/td>1000\u00a3<\/sup><\/td>17<\/td>0.9977<\/td>–<\/td>–<\/td>94<\/td>11<\/td>112<\/td>4<\/td>106<\/td>6<\/td><\/tr>
Spinetoram – spinosyn L (20%)d<\/sup><\/td>3000\u00a7<\/sup><\/td>2<\/td>0.9993<\/td>107<\/td>10<\/td>109<\/td>4<\/td>107<\/td>3<\/td>102<\/td>1<\/td><\/tr>
Piperonyl Butoxide<\/td>8000<\/td>5<\/td>0.9998<\/td>110<\/td>5<\/td>99<\/td>2<\/td>94<\/td>3<\/td>95<\/td>5<\/td><\/tr>
Chlorpyrifos*<\/td><LOD<\/td>20<\/td>0.9995<\/td>–<\/td>–<\/td>103<\/td>9<\/td>106<\/td>4<\/td>104<\/td>5<\/td><\/tr>
Hexythiazox<\/td>2000<\/td>10<\/td>0.9975<\/td>104<\/td>15<\/td>102<\/td>3<\/td>107<\/td>4<\/td>106<\/td>5<\/td><\/tr>
Etoxazole<\/td>1500<\/td>5<\/td>0.9995<\/td>103<\/td>4<\/td>104<\/td>2<\/td>103<\/td>1<\/td>100<\/td>1<\/td><\/tr>
Spiromesifen<\/td>12,000<\/td>5<\/td>0.9992<\/td>98<\/td>8<\/td>109<\/td>7<\/td>111<\/td>2<\/td>102<\/td>2<\/td><\/tr>
Pyrethrin I (54%)e<\/sup><\/td>1000\u00a3<\/sup><\/td>11<\/td>0.9977<\/td>–<\/td>–<\/td>98<\/td>5<\/td>105<\/td>12<\/td>104<\/td>5<\/td><\/tr>
Cyfluthrin<\/td>1000<\/td>50<\/td>0.999<\/td>–<\/td>–<\/td>93<\/td>11<\/td>102<\/td>23<\/td>115<\/td>10<\/td><\/tr>
Cypermethrin<\/td>1000<\/td>50<\/td>0.9961<\/td>–<\/td>–<\/td>115<\/td>11<\/td>98<\/td>18<\/td>104<\/td>6<\/td><\/tr>
(E)-Fenpyroximate<\/td>2000<\/td>5<\/td>0.9995<\/td>102<\/td>9<\/td>109<\/td>3<\/td>109<\/td>2<\/td>105<\/td>2<\/td><\/tr>
Permethrin-trans<\/em> (59%)h<\/sup><\/td>20,000\u00a2<\/sup><\/td>12<\/td>0.9994<\/td>–<\/td>–<\/td>99<\/td>8<\/td>104<\/td>5<\/td>101<\/td>3<\/td><\/tr>
Permethrin-cis<\/em> (41%)g<\/sup><\/td>20,000\u00a2<\/sup><\/td>8<\/td>0.9996<\/td>95<\/td>5<\/td>104<\/td>5<\/td>103<\/td>4<\/td>101<\/td>3<\/td><\/tr>
Avermectin B1a<\/td>300<\/td>50<\/td>0.9988<\/td>–<\/td>–<\/td>114<\/td>3<\/td>108<\/td>2<\/td>105<\/td>2<\/td><\/tr>
Etofenprox*<\/td><LOD<\/td>5<\/td>0.9994<\/td>104<\/td>7<\/td>107<\/td>1<\/td>106<\/td>2<\/td>103<\/td>1<\/td><\/tr>
Bifenthrin<\/td>500<\/td>5<\/td>0.999<\/td>99<\/td>5<\/td>103<\/td>2<\/td>108<\/td>6<\/td>104<\/td>2<\/td><\/tr>
Acequinocyl<\/td>4000<\/td>10<\/td>0.9997<\/td>104<\/td>7<\/td>109<\/td>3<\/td>108<\/td>3<\/td>106<\/td>2<\/td><\/tr>
Quintozene (PCNB) (GC)<\/td>200<\/td>10<\/td>0.9966<\/td>110<\/td>14<\/td>102<\/td>5<\/td>101<\/td>1<\/td>97<\/td>3<\/td><\/tr>
Methyl parathion (GC)*<\/td><LOD<\/td>5<\/td>0.9934<\/td>89<\/td>10<\/td>89<\/td>5<\/td>87<\/td>3<\/td>89<\/td>6<\/td><\/tr>
Captan (GC)<\/td>5000<\/td>10<\/td>0.9924<\/td>110<\/td>14<\/td>96<\/td>10<\/td>94<\/td>18<\/td>92<\/td>7<\/td><\/tr>
Chlordane (GC)*<\/td><LOD<\/td>20<\/td>0.9913<\/td>–<\/td>–<\/td>105<\/td>9<\/td>93<\/td>8<\/td>85<\/td>10<\/td><\/tr>
Chlorfenapyr (GC)*<\/td><LOD<\/td>10<\/td>0.9924<\/td>97<\/td>9<\/td>90<\/td>19<\/td>89<\/td>6<\/td>85<\/td>13<\/td><\/tr>
Cyfluthrin (GC)<\/td>1000<\/td>5<\/td>0.9935<\/td>107<\/td>10<\/td>92<\/td>18<\/td>91<\/td>7<\/td>89<\/td>11<\/td><\/tr>
Cypermethrin (GC)<\/td>1000<\/td>5<\/td>0.9938<\/td>95<\/td>9<\/td>83<\/td>17<\/td>97<\/td>15<\/td>93<\/td>9<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

*Pesticides de cat\u00e9gorie I, LQ\u2264100 ng\/g
a<\/sup>Spinosad- spinosyn A: Conc. 1: 7 ng\/g; Conc. 2: 35.5 ng\/g; Conc. 3: 71 ng\/g; Conc. 4: 355 ng\/g
b<\/sup>Spinosad – spinosyn D: Conc. 1: 3 ng\/g; conc. 2: 14.5 ng\/g; Conc. 3: 29 ng\/g; Conc. 4: 145 ng\/g
c<\/sup>Spinetoram – spinosyn J: Conc. 1: 8 ng\/g; Conc. 2: 40 ng\/g; Conc. 3: 80 ng\/g; Conc. 4: 400 ng\/g
d<\/sup>Spinetoram – spinosyn L: Conc. 1: 2 ng\/g; Conc. 2: 10 ng\/g; Conc. 3: 20 ng\/g; Conc. 4: 100 ng\/g
e<\/sup>Pyrethrin I: Conc. 1: 5 ng\/g; Conc. 2: 27 ng\/g; Conc. 3: 54 ng\/g; Conc. 4: 270 ng\/g
f<\/sup>Pyrethrin II: Conc. 1: 3 ng\/g; Conc. 2: 17 ng\/g; Conc. 3: 34 ng\/g; Conc. 4: 170 ng\/g
g<\/sup>Permethrin-cis<\/em>: Conc. 1: 4 ng\/g; Conc. 2: 20.5 ng\/g; Conc. 3: 41 ng\/g; Conc. 4: 205 ng\/g
h<\/sup>Permethrin-trans<\/em>: Conc. 1: 6 ng\/g; Conc. 2: 29.5 ng\/g; Conc. 3: 59 ng\/g; Conc. 4: 295 ng\/g
#<\/sup>Le total en aflatoxines B1, B2, G1 et G2 ne doit pas exc\u00e9der 20 ng\/g.
\u00a5<\/sup>Le spinosad total ne doit pas exc\u00e9der 3 000 ng\/g.
\u00a7<\/sup>Le spin\u00e9torame total ne doit pas exc\u00e9der 3 000ng\/g.
\u00a3<\/sup> Le total en pyr\u00e9thrines ne doit pas exc\u00e9der 1 000ng\/g.
\u00a2<\/sup>Le total en perm\u00e9thrines ne doit pas exc\u00e9der 20 000ng\/g.<\/p>\n\n\n\n

Tableau XI :<\/strong> Lin\u00e9arit\u00e9  pour les cannabino\u00efdes dan les bonbons g\u00e9lifi\u00e9s au cannabis.<\/p>\n\n\n\n

Cannabino\u00efdes<\/strong><\/td>Temps de r\u00e9tention<\/strong><\/td>R2<\/sup><\/strong><\/td>Equation<\/strong><\/td><\/tr>
Cannabidiolic acid (CBDA)<\/td>2.142<\/td>0.9993<\/td>y = 2.08e+004x + 1.03e+003<\/td><\/tr>
Cannabigerol (CBG)<\/td>2.405<\/td>0.9981<\/td>y = 1.16e+004x + 1.85e+003<\/td><\/tr>
Cannabidiol (CBD)<\/td>2.535<\/td>0.9972<\/td>y = 1.17e+004x + 1.42e+003<\/td><\/tr>
Cannabinol (CBN)<\/td>3.776<\/td>0.9980<\/td>y = 2.70e+004x + 6.14e+004<\/td><\/tr>
Delta-9-tetrahydrocannabinol (Delta-9-THC)<\/td>4.753<\/td>0.9970<\/td>y = 1.06e+004x + 7.29e+003<\/td><\/tr>
Tetrahydrocannabinolic acid (THCA)<\/td>6.279<\/td>0.9986<\/td>y = 1.78e+004x – 1.28e+003<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

Tableau XII : <\/strong>Exactitude et pr\u00e9cision pour les cannabino\u00efdes dans les bonbons g\u00e9lifi\u00e9s au cannabis.<\/p>\n\n\n\n

Cannabino\u00efdes\/niveau de dopage<\/strong><\/td>Concentration de l\u2019extrait dilu\u00e9 (ppm)<\/strong><\/td>Moyenne (ppm)<\/strong><\/td>SD<\/strong><\/td>RSD (%)<\/strong><\/td>Concentration de l\u2019extrait non dilu\u00e9 (ppm)<\/strong><\/td>Concentration estim\u00e9e de l\u2019\u00e9chantillon (mg\/g)<\/strong><\/td>Exactitude (%)<\/strong><\/td>Pourcentage d’erreur<\/strong><\/td><\/tr>
Bonbon dop\u00e9 \u00e0 0.2 mg\/g<\/strong><\/td>Replicate 1<\/strong><\/td>Replicate 2<\/strong><\/td><\/tr>
Cannabidiolic acid (CBDA)<\/td>4.2<\/td>4.4<\/td>4.3<\/td>0.1<\/td>3<\/td>43<\/td>0.2<\/td>107<\/td>7<\/td><\/tr>
Cannabigerol (CBG)<\/td>4.0<\/td>3.9<\/td>4.0<\/td>0.1<\/td>2<\/td>40<\/td>0.2<\/td>99<\/td>1<\/td><\/tr>
Cannabidiol (CBD)<\/td>4.1<\/td>4.2<\/td>4.1<\/td>0.1<\/td>2<\/td>41<\/td>0.2<\/td>103<\/td>3<\/td><\/tr>
Cannabinol (CBN)<\/td>4.0<\/td>4.1<\/td>4.1<\/td>0.1<\/td>3<\/td>41<\/td>0.2<\/td>101<\/td>1<\/td><\/tr>
Delta-9 tetrahydrocannabinol (Delta 9 THC)<\/td>4.0<\/td>4.2<\/td>4.1<\/td>0.1<\/td>3<\/td>41<\/td>0.2<\/td>103<\/td>3<\/td><\/tr>
Tetrahydrocannabinolic acid (THCA)<\/td>4.1<\/td>4.3<\/td>4.2<\/td>0.1<\/td>3<\/td>42<\/td>0.2<\/td>105<\/td>5<\/td><\/tr>
 <\/td> <\/td> <\/td> <\/td> <\/td> <\/td> <\/td> <\/td> <\/td> <\/td><\/tr>
Gummy spiked at 0.5 mg\/g<\/strong><\/td> <\/td> <\/td> <\/td> <\/td> <\/td> <\/td> <\/td> <\/td> <\/td><\/tr>
Cannabidiolic acid (CBDA)<\/td>10.4<\/td>10.7<\/td>10.6<\/td>0.2<\/td>2<\/td>106<\/td>0.5<\/td>106<\/td>6<\/td><\/tr>
Cannabigerol (CBG)<\/td>9.5<\/td>10.3<\/td>9.9<\/td>0.5<\/td>5<\/td>99<\/td>0.5<\/td>99<\/td>1<\/td><\/tr>
Cannabidiol (CBD)<\/td>9.8<\/td>10.6<\/td>10.2<\/td>0.5<\/td>5<\/td>102<\/td>0.5<\/td>102<\/td>2<\/td><\/tr>
Cannabinol (CBN)<\/td>9.8<\/td>10.3<\/td>10.0<\/td>0.4<\/td>4<\/td>100<\/td>0.5<\/td>100<\/td>0<\/td><\/tr>
Delta-9-tetrahydrocannabinol (Delta-9-THC)<\/td>9.9<\/td>10.3<\/td>10.1<\/td>0.3<\/td>3<\/td>101<\/td>0.5<\/td>101<\/td>1<\/td><\/tr>
Tetrahydrocannabinolic acid (THCA)<\/td>10.3<\/td>9.9<\/td>10.1<\/td>0.2<\/td>2<\/td>101<\/td>0.5<\/td>101<\/td>1<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n
Figure 2 :\u00a0<\/strong>Chromatogramme LC-MS\/MS d\u2019un extrait obtenu par dopage d\u2019un \u00e9chantillon blanc avec des pesticides et des mycotoxines \u00e0 100 ng\/g.<\/div>
\n
\"California<\/div>

LC_GN0666<\/p>

Peaks<\/h4>\n
<\/th>Peaks<\/th>tR<\/sub> (min)<\/th>Precursor Ion<\/th>Product Ion 1<\/th>Product Ion 2<\/th>Polarity<\/th><\/tr><\/thead>\n
1.<\/td>Daminozide-d6<\/td>0.7<\/td>167.0<\/td>149.3<\/td>49.3<\/td>+<\/td><\/tr>\n
2.<\/td>Daminozide<\/a><\/td>0.7<\/td>161.1<\/td>44.1<\/td>143.2<\/td>+<\/td><\/tr>\n
3.<\/td>Acephate<\/a><\/td>1.7<\/td>184.0<\/td>143.1<\/td>95.1<\/td>+<\/td><\/tr>\n
4.<\/td>Oxamyl<\/a><\/td>2.0<\/td>237.1<\/td>72.1<\/td>90.1<\/td>+<\/td><\/tr>\n
5.<\/td>Flonicamid<\/a><\/td>2.1<\/td>230.1<\/td>203.1<\/td>174.1<\/td>+<\/td><\/tr>\n
6.<\/td>Methomyl<\/a><\/td>2.1<\/td>163.1<\/td>88.1<\/td>106.1<\/td>+<\/td><\/tr>\n
7.<\/td>Thiamethoxam<\/a><\/td>2.1<\/td>292.0<\/td>211.1<\/td>181.1<\/td>+<\/td><\/tr>\n
8.<\/td>Imidacloprid<\/a><\/td>2.3<\/td>256.1<\/td>209.1<\/td>175.1<\/td>+<\/td><\/tr>\n
9.<\/td>Mevinphos<\/a><\/td>2.4<\/td>225.1<\/td>127.1<\/td>193.2<\/td>+<\/td><\/tr>\n
10.<\/td>Acetamiprid<\/a><\/td>2.4<\/td>223.0<\/td>126.1<\/td>56.1<\/td>+<\/td><\/tr>\n
11.<\/td>Dimethoathe-d6<\/td>2.4<\/td>236.1<\/td>205.1<\/td>–<\/td>+<\/td><\/tr>\n
12.<\/td>Dimethoate<\/a><\/td>2.4<\/td>230.0<\/td>199.1<\/td>125.1<\/td>+<\/td><\/tr>\n
13.<\/td>Thiacloprid<\/a><\/td>2.5<\/td>253.0<\/td>126.0<\/td>90.1<\/td>+<\/td><\/tr>\n
14.<\/td>Aflatoxin G2<\/a><\/td>2.5<\/td>331.2<\/td>189.3<\/td>115.2<\/td>+<\/td><\/tr>\n
15.<\/td>Aflatoxin G1<\/a><\/td>2.5<\/td>329.2<\/td>243.2<\/td>215.3<\/td>+<\/td><\/tr>\n
16.<\/td>Aldicarb<\/a><\/td>2.6<\/td>116.0<\/td>89.2<\/td>70.2<\/td>+<\/td><\/tr>\n
17.<\/td>Aflatoxin B2<\/a><\/td>2.6<\/td>315.3<\/td>287.2<\/td>243.3<\/td>+<\/td><\/tr>\n
18.<\/td>Dichlorvos<\/a><\/td>2.7<\/td>220.9<\/td>109.1<\/td>79.2<\/td>+<\/td><\/tr>\n
19.<\/td>Dichlorvos-d6<\/td>2.7<\/td>227.0<\/td>115.1<\/td>–<\/td>+<\/td><\/tr>\n
20.<\/td>Aflatoxin B1<\/a><\/td>2.7<\/td>313.2<\/td>241.2<\/td>128.2<\/td>+<\/td><\/tr>\n
21.<\/td>Imazalil<\/a><\/td>2.7<\/td>297.0<\/td>159.0<\/td>201.0<\/td>+<\/td><\/tr>\n
22.<\/td>Carbofuran<\/a><\/td>2.7<\/td>222.1<\/td>123.1<\/td>165.2<\/td>+<\/td><\/tr>\n
23.<\/td>Propoxur<\/a><\/td>2.7<\/td>210.1<\/td>111.1<\/td>93.1<\/td>+<\/td><\/tr>\n
24.<\/td>Carbaryl-d7<\/td>2.8<\/td>209.2<\/td>152.2<\/td>–<\/td>+<\/td><\/tr>\n
25.<\/td>Carbaryl<\/a><\/td>2.8<\/td>202.1<\/td>145.1<\/td>127.1<\/td>+<\/td><\/tr>\n
26.<\/td>Diuron-d6<\/td>3.0<\/td>239.1<\/td>78.2<\/td>–<\/td>+<\/td><\/tr>\n
27.<\/td>Atrazine-d5<\/a><\/td>3.0<\/td>221.2<\/td>179.1<\/td>–<\/td>+<\/td><\/tr>\n
28.<\/td>Naled<\/a><\/td>3.1<\/td>397.8<\/td>127.1<\/td>109.1<\/td>+<\/td><\/tr>\n
29.<\/td>Metalaxyl<\/a><\/td>3.1<\/td>280.2<\/td>220.2<\/td>192.2<\/td>+<\/td><\/tr>\n
30.<\/td>Spiroxamine<\/a><\/td>3.1<\/td>298.3<\/td>144.2<\/td>100.2<\/td>+<\/td><\/tr>\n
31.<\/td>Chlorantraniliprole<\/a><\/td>3.2<\/td>483.9<\/td>452.9<\/td>285.9<\/td>+<\/td><\/tr>\n
32.<\/td>Phosmet<\/a><\/td>3.2<\/td>318.0<\/td>160.1<\/td>77.2<\/td>+<\/td><\/tr>\n
33.<\/td>Azoxystrobin<\/a><\/td>3.3<\/td>404.0<\/td>372.1<\/td>344.1<\/td>+<\/td><\/tr>\n
34.<\/td>Linuron-d6<\/a><\/td>3.3<\/td>255.1<\/td>160.1<\/td>–<\/td>+<\/td><\/tr>\n
35.<\/td>Fludioxonil<\/a><\/td>3.4<\/td>247.0<\/td>180.0<\/td>126.0<\/td>–<\/td><\/tr>\n
36.<\/td>Methiocarb<\/a><\/td>3.4<\/td>226.1<\/td>169.1<\/td>121.1<\/td>+<\/td><\/tr>\n
37.<\/td>Dimethomorph<\/a><\/td>3.5<\/td>388.2<\/td>301.2<\/td>165.3<\/td>+<\/td><\/tr>\n
38.<\/td>Boscalid<\/a><\/td>3.5<\/td>342.9<\/td>307.1<\/td>140.1<\/td>+<\/td><\/tr>\n
39.<\/td>Paclobutrazol<\/a><\/td>3.6<\/td>294.3<\/td>70.1<\/td>125.1<\/td>+<\/td><\/tr>\n
40.<\/td>Malathion<\/a><\/td>3.6<\/td>331.0<\/td>127.2<\/td>285.2<\/td>+<\/td><\/tr>\n
41.<\/td>Myclobutanil<\/a><\/td>3.7<\/td>289.1<\/td>70.1<\/td>125.1<\/td>+<\/td><\/tr>\n
42.<\/td>Bifenazate<\/a><\/td>3.7<\/td>301.0<\/td>198.1<\/td>170.2<\/td>+<\/td><\/tr>\n
43.<\/td>Ochratoxin A<\/a><\/td>3.8<\/td>404.2<\/td>239.1<\/td>358.3<\/td>+<\/td><\/tr>\n
44.<\/td>Fenhexamid<\/a><\/td>3.9<\/td>302.1<\/td>97.1<\/td>55.2<\/td>+<\/td><\/tr>\n
45.<\/td>Spirotetramat<\/a><\/td>4.0<\/td>374.2<\/td>302.1<\/td>216.1<\/td>+<\/td><\/tr>\n
46.<\/td>Ethoprophos<\/a><\/td>4.1<\/td>243.1<\/td>131.1<\/td>97.1<\/td>+<\/td><\/tr>\n
47.<\/td>Fipronil<\/a><\/td>4.1<\/td>436.8<\/td>331.8<\/td>251.9<\/td>–<\/td><\/tr>\n
48.<\/td>Fenoxycarb<\/a><\/td>4.2<\/td>302.1<\/td>88.1<\/td>116.1<\/td>+<\/td><\/tr>\n
49.<\/td>Kresoxim-methyl<\/a><\/td>4.4<\/td>314.2<\/td>267.2<\/td>222.2<\/td>+<\/td><\/tr>\n
50.<\/td>Tebuconazole<\/a><\/td>4.4<\/td>308.1<\/td>70.1<\/td>125.1<\/td>+<\/td><\/tr>\n
51.<\/td>Diazinon-d10 <\/td>4.6<\/td>315.2<\/td>170.2<\/td>–<\/td>+<\/td><\/tr>\n
52.<\/td>Spinosyn A (Spinosad)<\/a><\/td>4.6<\/td>732.4<\/td>142.2<\/td>98.1<\/td>+<\/td><\/tr>\n
53.<\/td>Diazinon<\/a><\/td>4.6<\/td>305.1<\/td>169.2<\/td>153.2<\/td>+<\/td><\/tr>\n
54.<\/td>Coumaphos<\/a><\/td>4.7<\/td>363.1<\/td>227.1<\/td>307.1<\/td>+<\/td><\/tr>\n
55.<\/td>Pyridaben<\/a><\/td>4.7<\/td>365.1<\/td>309.2<\/td>147.2<\/td>+<\/td><\/tr>\n
56.<\/td>Propiconazole<\/a><\/td>4.7<\/td>342.0<\/td>159.0<\/td>69.2<\/td>+<\/td><\/tr>\n
57.<\/td>Clofentezine<\/a><\/td>4.8<\/td>303.0<\/td>138.1<\/td>102.1<\/td>+<\/td><\/tr>\n
58.<\/td>Spinosyn D (Spinosad)<\/a><\/td>5.0<\/td>746.5<\/td>142.3<\/td>98.4<\/td>+<\/td><\/tr>\n
59.<\/td>Spinosyn J (Spinetoram)<\/a><\/td>5.1<\/td>748.5<\/td>142.3<\/td>98.3<\/td>+<\/td><\/tr>\n
60.<\/td>Trifloxystrobin<\/a><\/td>5.3<\/td>409.2<\/td>186.1<\/td>145.1<\/td>+<\/td><\/tr>\n
61.<\/td>Prallethrin<\/a><\/td>5.3<\/td>301.2<\/td>123.2<\/td>105.2<\/td>+<\/td><\/tr>\n
62.<\/td>Pyrethrin II<\/a><\/td>5.5<\/td>373.1<\/td>161.1<\/td>133.2<\/td>+<\/td><\/tr>\n
63.<\/td>Spinosyn L (Spinetoram)<\/a><\/td>5.6<\/td>760.5<\/td>142.2<\/td>98.1<\/td>+<\/td><\/tr>\n
64.<\/td>Piperonyl butoxide<\/a><\/td>6.0<\/td>356.3<\/td>177.2<\/td>119.2<\/td>+<\/td><\/tr>\n
65.<\/td>Chlorpyrifos<\/a><\/td>6.1<\/td>349.9<\/td>198.0<\/td>97.1<\/td>+<\/td><\/tr>\n
66.<\/td>Hexythiazox<\/a><\/td>6.2<\/td>353.1<\/td>228.1<\/td>168.1<\/td>+<\/td><\/tr>\n
67.<\/td>Etoxazole<\/a><\/td>6.6<\/td>360.2<\/td>141.1<\/td>304.2<\/td>+<\/td><\/tr>\n
68.<\/td>Spiromesifen<\/a><\/td>6.7<\/td>273.2<\/td>255.2<\/td>187.2<\/td>+<\/td><\/tr>\n
69.<\/td>Pyrethrin I<\/a><\/td>6.9<\/td>329.2<\/td>161.2<\/td>105.2<\/td>+<\/td><\/tr>\n
70.<\/td>Cyfluthrin (qualifier)<\/a><\/td>6.9<\/td>453.1<\/td>193.2<\/td>–<\/td>+<\/td><\/tr>\n
71.<\/td>Cyfluthrin<\/a><\/td>6.9<\/td>451.1<\/td>191.2<\/td>–<\/td>+<\/td><\/tr>\n
72.<\/td>Cypermethrin<\/a><\/td>7.1<\/td>433.1<\/td>191.0<\/td>416.0<\/td>+<\/td><\/tr>\n
73.<\/td>(E)-Fenpyroximate<\/a><\/td>7.1<\/td>422.2<\/td>366.1<\/td>138.1<\/td>+<\/td><\/tr>\n
74.<\/td>trans-Permethrin<\/a><\/td>7.6<\/td>408.3<\/td>183.2<\/td>355.1<\/td>+<\/td><\/tr>\n
75.<\/td>cis-Permethrin<\/a><\/td>7.9<\/td>408.3<\/td>183.2<\/td>355.1<\/td>+<\/td><\/tr>\n
76.<\/td>Avermectin B1a<\/a><\/td>7.9<\/td>890.5<\/td>305.4<\/td>567.4<\/td>+<\/td><\/tr>\n
77.<\/td>Etofenprox<\/a><\/td>8.0<\/td>394.3<\/td>177.2<\/td>359.3<\/td>+<\/td><\/tr>\n
78.<\/td>Bifenthrin<\/a><\/td>8.2<\/td>440.0<\/td>181.2<\/td>166.2<\/td>+<\/td><\/tr>\n
79.<\/td>Acequinocyl (precursor ion 1)<\/a><\/td>9.4<\/td>402.3<\/td>343.2<\/td>189.0<\/td>+<\/td><\/tr>\n
80.<\/td>Acequinocyl (precursor ion 2)<\/a><\/td>9.4<\/td>386.0<\/td>344.2<\/td>189.1<\/td>+<\/td><\/tr>\n<\/tbody><\/table><\/div>

Conditions<\/h4>
Column<\/th>Raptor ARC-18 (cat.# 9314A12<\/a>)<\/td><\/tr>
Dimensions:<\/th>100 mm x 2.1 mm ID<\/td><\/tr>
Particle Size:<\/th>2.7 \u00b5m<\/td><\/tr>
Pore Size:<\/th>90 \u00c5<\/td><\/tr>
<\/td>
Guard Column:<\/th>Raptor ARC-18 EXP guard column cartridge 5 mm, 2.1 mm ID, 2.7 \u00b5m (cat.# 9314A0252<\/a>)<\/td><\/tr>
Temp.:<\/th>40 \u00b0C<\/td><\/tr>
Standard\/Sample<\/th><\/td><\/tr>
<\/td>California pesticide standard #1 (cat.# 34124<\/a>)<\/td><\/tr>
<\/td>California pesticide standard #2 (cat.# 34125<\/a>)<\/td><\/tr>
<\/td>California pesticide standard #3 (cat.# 34126<\/a>)<\/td><\/tr>
<\/td>California pesticide standard #4 (cat.# 34127<\/a>)<\/td><\/tr>
<\/td>California pesticide standard #5 (cat.# 34128<\/a>)<\/td><\/tr>
<\/td>California pesticide standard #6 (cat.# 34129<\/a>)<\/td><\/tr>
<\/td>Dimethoate-d6 (cat.# 31988<\/a>)<\/td><\/tr>
<\/td>Dichlorvos-d6 (cat.# 31987<\/a>)<\/td><\/tr>
<\/td>Carbaryl-d7 (cat.# 31985<\/a>)<\/td><\/tr>
<\/td>Diazinon-d10 (cat.# 31986<\/a>)<\/td><\/tr>
<\/td>Atrazine-d5 (cat.# 31984<\/a>)<\/td><\/tr>
<\/td>Diuron-d6 (cat.# 31989<\/a>)<\/td><\/tr>
<\/td>Liuron-d6 (cat.# 31990<\/a>)<\/td><\/tr>
<\/td>Aflatoxins standard (cat.# 34121<\/a>)<\/td><\/tr>
<\/td>Ochratoxin A (cat.# 34122<\/a>)<\/td><\/tr>
<\/td>Compounds not present in these mixes were obtained separately.<\/td><\/tr>\n
Diluent:<\/th>75:25 Acetonitrile:water<\/td><\/tr>
Conc.:<\/th>3.75-15 ng\/mL (Expected concentration range in extract of gummy initially spiked at 100 ng\/g.)<\/td><\/tr><\/td><\/tr>
Inj. Vol.:<\/th>2 \u00b5L <\/td><\/tr>
Mobile Phase<\/th><\/td><\/tr>
A:<\/th>Water, 2 mM ammonium formate, 0.1% formic acid <\/td><\/tr>
B:<\/th>Methanol, 2 mM ammonium formate, 0.1% formic acid <\/td><\/tr>
<\/td>
Time (min)<\/th>Flow (mL\/min)<\/th>%A<\/th>%B<\/th><\/tr><\/thead>
0.00<\/td>0.5<\/td>95<\/td>5<\/td><\/tr>
1.5<\/td>0.5<\/td>35<\/td>65<\/td><\/tr>
8.5<\/td>0.5<\/td>5<\/td>95<\/td><\/tr>
9.5<\/td>0.5<\/td>0<\/td>100<\/td><\/tr>
10.5<\/td>0.5<\/td>0<\/td>100<\/td><\/tr>
10.6<\/td>0.5<\/td>95<\/td>5<\/td><\/tr>
12.0<\/td>0.5<\/td>95<\/td>5<\/td><\/tr><\/tbody><\/table><\/td><\/tr><\/table>
Detector<\/th>MS\/MS<\/td><\/tr>
Ion Mode:<\/th>ESI+\/ESI- <\/td><\/tr>
Mode:<\/th>MRM <\/td><\/tr>
Instrument<\/th>UHPLC<\/td><\/tr>
Sample Preparation<\/th>Gummies were manually chopped into small pieces, and 1 g of sample was weighed in a 50 mL polypropylene tube. The sample was mixed with 5 mL of water and then vigorously vortexed until all gummy pieces were fully solubilized. The sample was fortified with pesticides and mycotoxins at 100 ng\/g. A mix of internal standards was added at 200 ng\/g. The spiked sample was further vortexed for 30 sec. 5 mL of acetonitrile acidified with 1% acetic acid was added to the sample, and this was followed by a 30 sec vortex agitation. Then, a pouch of European EN 15662 QuEChERS extraction salts (cat.# 25849<\/a>) was added to the sample. The sample was vortexed for 30 sec and then centrifuged for 5 min. 750 \u00b5L of organic extract was mixed with 250 \u00b5L of water. 2 \u03bcL of final extract was injected into the LC-MS\/MS system.<\/td><\/tr>
Notes<\/th>Want even better performance when analyzing metal-sensitive compounds? Check out Inert LC columns at www.restek.com\/inert<\/a>.<\/td><\/tr><\/table><\/div><\/div><\/div>
<\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n<\/div><\/div><\/div>\n\n
Figure 3 :<\/strong>\u00a0Chromatogramme GC-MS\/MS d\u2019un extrait obtenu par dopage d\u2019un \u00e9chantillon blanc avec des pesticides et des mycotoxines \u00e0 100 ng\/g.<\/div>
\n
\"GC<\/div>

GC_GN1207<\/p>

Peaks<\/h4>\n
<\/th>Peaks<\/th>tR<\/sub> (min)<\/th>Polarity<\/th>Precursor Ion<\/th>Product Ion<\/th>Transition Type<\/th><\/tr><\/thead>\n
1.<\/td>Atrazine-d5<\/a><\/td>6.82<\/td>Positive<\/td>220.0<\/td>58.0<\/td>Quantifier<\/td><\/tr>\n
2.<\/td>Atrazine-d5<\/a><\/td>6.82<\/td>Positive<\/td>205.0<\/td>127.0<\/td>Qualifier<\/td><\/tr>\n
3.<\/td>Diazinon-d10 (diethyl-d10)<\/td>7.01<\/td>Positive<\/td>183.0<\/td>139.0<\/td>Quantifier<\/td><\/tr>\n
4.<\/td>Diazinon-d10 (diethyl-d10)<\/td>7.01<\/td>Positive<\/td>183.0<\/td>168.0<\/td>Qualifier<\/td><\/tr>\n
5.<\/td>Quintozene<\/a><\/td>7.03<\/td>Positive<\/td>294.9<\/td>236.9<\/td>Quantifier<\/td><\/tr>\n
6.<\/td>Quintozene<\/a><\/td>7.03<\/td>Positive<\/td>236.8<\/td>118.9<\/td>Qualifier<\/td><\/tr>\n
7.<\/td>Methyl parathion<\/a><\/td>7.50<\/td>Positive<\/td>263.0<\/td>109.0<\/td>Quantifier<\/td><\/tr>\n
8.<\/td>Methyl parathion<\/a><\/td>7.50<\/td>Positive<\/td>263.0<\/td>79.0<\/td>Qualifier<\/td><\/tr>\n
9.<\/td>Captan<\/a><\/td>8.37<\/td>Positive<\/td>184.0<\/td>149.1<\/td>Quantifier<\/td><\/tr>\n
10.<\/td>Captan<\/a><\/td>8.37<\/td>Positive<\/td>184.0<\/td>134.1<\/td>Qualifier<\/td><\/tr>\n
11.<\/td>trans-Chlordane<\/a><\/td>8.41<\/td>Positive<\/td>271.9<\/td>237.0<\/td>Quantifier<\/td><\/tr>\n
12.<\/td>trans-Chlordane<\/a><\/td>8.41<\/td>Positive<\/td>372.9<\/td>265.9<\/td>Qualifier<\/td><\/tr>\n
13.<\/td>cis-Chlordane<\/a><\/td>8.53<\/td>Positive<\/td>372.9<\/td>265.9<\/td>Quantifier<\/td><\/tr>\n
14.<\/td>cis-Chlordane<\/a><\/td>8.53<\/td>Positive<\/td>271.9<\/td>237.0<\/td>Qualifier<\/td><\/tr>\n
15.<\/td>Chlorfenapyr<\/a><\/td>8.80<\/td>Positive<\/td>247.1<\/td>227.1<\/td>Quantifier<\/td><\/tr>\n
16.<\/td>Chlorfenapyr<\/a><\/td>8.80<\/td>Positive<\/td>59.1<\/td>31.1<\/td>Qualifier<\/td><\/tr>\n
17.<\/td>Cyfluthrin<\/a><\/td>10.61<\/td>Positive<\/td>226.0<\/td>206.0<\/td>Quantifier<\/td><\/tr>\n
18.<\/td>Cyfluthrin<\/a><\/td>10.61<\/td>Positive<\/td>163.0<\/td>127.0<\/td>Qualifier<\/td><\/tr>\n
19.<\/td>Cypermethrin<\/a><\/td>10.87<\/td>Positive<\/td>163.0<\/td>127.1<\/td>Quantifier<\/td><\/tr>\n
20.<\/td>Cypermethrin<\/a><\/td>10.87<\/td>Positive<\/td>181.1<\/td>152.1<\/td>Qualifier<\/td><\/tr>\n<\/tbody><\/table><\/div>

Conditions<\/h4>
Column<\/th>Rxi-5ms, 30 m, 0.25 mm ID, 0.25 \u00b5m (cat.# 13423<\/a>)<\/td><\/tr>
Standard\/Sample<\/th><\/td><\/tr>
<\/td>California pesticide standard #1 (cat.# 34124<\/a>)<\/td><\/tr>
<\/td>California pesticide standard #2 (cat.# 34125<\/a>)<\/td><\/tr>
<\/td>California pesticide standard #3 (cat.# 34126<\/a>)<\/td><\/tr>
<\/td>California pesticide standard #4 (cat.# 34127<\/a>)<\/td><\/tr>
<\/td>California pesticide standard #5 (cat.# 34128<\/a>)<\/td><\/tr>
<\/td>California pesticide standard #6 (cat.# 34129<\/a>)<\/td><\/tr>
<\/td>Atrazine-d5 (cat.# 31984<\/a>)<\/td><\/tr>
<\/td>Diazinon-d10 (cat.# 31986<\/a>)<\/td><\/tr>\n
Diluent:<\/th>Acetonitrile <\/td><\/tr>
Conc.:<\/th>2.5-10 ng\/mL Expected concentration range in extract after extracting from gummy fortified at 100 ng\/g (final extract was diluted in half with acetonitrile).<\/td><\/tr>
Injection<\/th><\/td><\/tr>
Inj. Vol.:<\/th>1 \u00b5L splitless<\/td><\/tr>
Liner:<\/th>Topaz 4.0 mm ID single taper inlet liner w\/wool (cat.# 23447<\/a>)<\/td><\/tr>
Inj. Temp.:<\/th>250 \u00b0C<\/td><\/tr>
Purge Flow:<\/th>5 mL\/min<\/td><\/tr>
Oven<\/td><\/tr>
Oven Temp.:<\/th>90 °C (hold 1 min) to 310 °C at 25 °C\/min (hold 10 min)<\/td><\/tr>
Carrier Gas<\/th>He, constant flow<\/td><\/tr>
Flow Rate:<\/th>1.4 mL\/min<\/td><\/tr><\/table>
Detector<\/th>MS\/MS<\/td><\/tr>
Transfer Line Temp.:<\/th>290 \u00b0C<\/td><\/tr>
Analyzer Type:<\/th>Quadrupole <\/td><\/tr>
Source Temp.:<\/th>330 \u00b0C<\/td><\/tr>
Electron Energy:<\/th>70 eV<\/td><\/tr>
Tune Type:<\/th>PFTBA <\/td><\/tr>
Ionization Mode:<\/th>EI <\/td><\/tr>
Instrument<\/th>Thermo Scientific TSQ 8000 Triple Quadrupole GC-MS<\/td><\/tr>
Sample Preparation<\/th>Gummies were manually chopped into small pieces, and 1 g of sample was weighed in a 50 mL polypropylene tube. The sample was mixed with 5 mL of water and then vigorously vortexed until all gummy pieces were fully solubilized. The sample was fortified with pesticides and mycotoxins at 100 ng\/g. A mix of internal standards was added at 200 ng\/g. The spiked sample was further vortexed for 30 sec. 5 mL of acetonitrile acidified with 1% acetic acid was added to the sample, and this was followed by 30 sec vortex agitation. Then, a pouch of European EN 15662 QuEChERS extraction salts (cat.# 25849<\/a>) was added to the sample. The sample was vortexed for 30 sec and then centrifuged for 5 min. 1.9 mL of supernatant was transferred to a Q-sep QuEChERS dSPE tube containing pre-weighed magnesium sulfate, PSA, and GCB (cat.# 26217<\/a>). After vortexing and centrifuging, 500 \u03bcL of extract was mixed with 500 \u03bcL of acidified acetonitrile. 1 \u03bcL of final extract was injected into the GC-MS\/MS system.<\/td><\/tr><\/table><\/div><\/div><\/div>
<\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n<\/div><\/div><\/div>\n\n
Figure 4 :<\/strong>\u00a0Chromatogramme HPLC-UV d\u2019un extrait obtenu par dopage d\u2019un \u00e9chantillon blanc avec six cannabino\u00efdes \u00e0 0.2 mg\/g.<\/div>
\n
\"Cannabinoids<\/div>

LC_GN0667<\/p>

Peaks<\/h4>\n
<\/th>Peaks<\/th>tR<\/sub> (min)<\/th>mg\/g*<\/th><\/tr><\/thead>\n
1.<\/td>Cannabidiolic acid (CBDA)<\/a><\/td>2.142<\/td>0.2<\/td><\/tr>\n
2.<\/td>Cannabigerol (CBG)<\/a><\/td>2.405<\/td>0.2<\/td><\/tr>\n
3.<\/td>Cannabidiol (CBD)<\/a><\/td>2.535<\/td>0.2<\/td><\/tr>\n
4.<\/td>Cannabinol (CBN)<\/a><\/td>3.776<\/td>0.2<\/td><\/tr>\n
5.<\/td>\u03949-Tetrahydrocannabinol (\u03949-THC)<\/a><\/td>4.753<\/td>0.2<\/td><\/tr>\n
6.<\/td>Tetrahydrocannabinolic acid A (THCA-A)<\/a><\/td>6.279<\/td>0.2<\/td><\/tr>\n<\/tbody><\/table>
*Extract from a gummy sample initially spiked at 0.2 mg\/g.<\/div><\/div>

Conditions<\/h4>
Column<\/th>Raptor ARC-18 (cat.# 9314A62<\/a>)<\/td><\/tr>
Dimensions:<\/th>150 mm x 2.1 mm ID<\/td><\/tr>
Particle Size:<\/th>2.7 \u00b5m<\/td><\/tr>
Pore Size:<\/th>90 \u00c5<\/td><\/tr>
<\/td>
Guard Column:<\/th>Raptor ARC-18 EXP guard column cartridge 5 mm, 2.1 mm ID, 2.7 \u00b5m (cat.# 9314A0252<\/a>)<\/td><\/tr>
Temp.:<\/th>30 \u00b0C<\/td><\/tr>
Standard\/Sample<\/th><\/td><\/tr>
<\/td>Cannabinoids standard (cat.# 34014<\/a>)<\/td><\/tr>
<\/td>Cannabigerol (cat.# 34091<\/a>)<\/td><\/tr>
<\/td>d9-Tetrahydrocannabinol (cat.# 34067<\/a>)<\/td><\/tr>
<\/td>d9-Tetrahydrocannabinolic acid A (cat.# 34111<\/a>)<\/td><\/tr>\n
Diluent:<\/th>75:25 Acetonitrile:water<\/td><\/tr>
Conc.:<\/th> Expected concentration of 4 ppm in final extract from gummy initially spiked at 0.2 mg\/g.<\/td><\/tr><\/td><\/tr>
Inj. Vol.:<\/th>2 \u00b5L <\/td><\/tr>
Mobile Phase<\/th><\/td><\/tr>
A:<\/th>Water, 5 mM ammonium formate, 0.1% formic acid <\/td><\/tr>
B:<\/th>Acetonitrile, 0.1% formic acid <\/td><\/tr>
<\/td>
Time (min)<\/th>Flow (mL\/min)<\/th>%A<\/th>%B<\/th><\/tr><\/thead>
0.00<\/td>0.4<\/td>25<\/td>75<\/td><\/tr>
10.00<\/td>0.4<\/td>25<\/td>75<\/td><\/tr><\/tbody><\/table><\/td><\/tr><\/table>
Detector<\/th>UV\/Vis @ 228 nm<\/td><\/tr>
Instrument<\/th>UHPLC<\/td><\/tr>
Sample Preparation<\/th>Gummies were manually chopped into small pieces, and 1 g of sample was weighed in a 50 mL polypropylene tube. The sample was mixed with 5 mL of water and then vigorously vortexed until all gummy pieces were fully solubilized. The sample was fortified with cannabinoids at 0.2 mg\/g. The spiked sample was further vortexed for 30 sec. 5 mL of acetonitrile acidified with 1% acetic acid was added to the sample, and this was followed by 30 sec vortex agitation. Then, a pouch of European EN 15662 QuEChERS extraction salts (cat.# 25849<\/a>) was added to the sample. The sample was vortexed for 30 sec and then centrifuged for 5 min. 100 \u00b5L of organic extract was mixed with 900 \u00b5L of 75:25 acetonitrile:water. 2 \u00b5L of final extract was injected into the HPLC-UV system.<\/td><\/tr><\/table><\/div><\/div><\/div>
<\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n<\/div><\/div><\/div>\n\n\n
<\/div>\n\n\n\n

Conclusion<\/h2>\n\n\n\n

Une m\u00e9thode simple et efficace pour l’analyse des pesticides, des mycotoxines et des cannabino\u00efdes dans les bonbons g\u00e9lifi\u00e9s au cannabis a \u00e9t\u00e9 d\u00e9velopp\u00e9. Les conditions de pr\u00e9paration d\u2019\u00e9chantillons ont inclus l’homog\u00e9n\u00e9isation de la matrice (bonbons g\u00e9lifi\u00e9s en petits morceaux) avec de l’eau, l’extraction des analytes \u00e0 l’aide d’ac\u00e9tonitrile acidifi\u00e9 suivie d’une \u00e9tape de relargage \u00e0 l’aide de sels d’extraction QuEChERS Q-sep ; la dilution de l\u2019extrait (pour les contaminants et les cannabino\u00efdes susceptibles d’\u00eatre analys\u00e9s par LC-MS\/MS) ; et le nettoyage\/la purification dSPE \u00e0 l’aide de sulfate de magn\u00e9sium, de PSA et de GCB (pour les pesticides analysables par GC-MS\/MS). Des r\u00e9sultats satisfaisants en termes de LQ, de lin\u00e9arit\u00e9, d’exactitude et de pr\u00e9cision ont \u00e9t\u00e9 obtenus pour tous les contaminants cibles. De plus, nos donn\u00e9es ont d\u00e9montr\u00e9 que la m\u00e9thodologie propos\u00e9e convient aux analyses de puissance avec des valeurs d\u2019exactitude comprises entre 99 et 107 % pour les six cannabino\u00efdes r\u00e9pertori\u00e9s dans la r\u00e9glementation sur le cannabis de l’\u00c9tat de Californie. Dans l’ensemble, la m\u00e9thode pr\u00e9sent\u00e9e simplifie le travail des laboratoires d\u2019analyse de cannabis en permettant la quantification de plusieurs familles de compos\u00e9s dans des \u00e9chantillons de bonbons g\u00e9lifi\u00e9s \u00e0 l’aide d’un seul et unique extrait.<\/p>\n\n\n\n

R\u00e9f\u00e9rences<\/h2>\n\n\n\n
    \n
  1. Text of Regulations, Bureau of Cannabis Control, California Code of Regulations,\u00a0https:\/\/cannabis.ca.gov\/wp-content\/uploads\/sites\/13\/2019\/01\/Order-of-Adoption-Clean-Version-of-Text.pdf<\/a>, (accessed 8 November 2019).<\/li>\n\n\n\n
  2. X. Wang, D. Mackowsky, J. Searfoss, M. J. Telepchak, Determination of cannabinoid content and pesticide residues in cannabis edibles and beverages, Cannabis Sci. and Tech. (2018).\u00a0https:\/\/www.cannabissciencetech.com\/view\/determination-cannabinoid-content-and-pesticide-residues-cannabis-edibles-and-beverages<\/a>.<\/li>\n\n\n\n
  3. Fast, low-solvent analysis of cannabinoids increases lab productivity and decreases solvent costs<\/a>, Restek Corporation.<\/li>\n\n\n\n
  4. N. Reyes-Garces, C. Myers,\u00a0Analysis of pesticides and mycotoxins cannabis brownies<\/a>, Restek Corporation.<\/li>\n\n\n\n
  5. B. K. Matuszewski, M. L. Constanzer, C. M. Chavez-Eng, Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC\u2212MS\/MS, Anal. Chem. 75 (2003) 3019\u20133030.\u00a0https:\/\/pubs.acs.org\/doi\/10.1021\/ac020361s<\/a><\/li>\n<\/ol>\n\n\n\n
    <\/div>\n\n\n
    \n

    Products Mentioned<\/h3>\n
    \n
    \n
    \n
    \n Catalog No. 25846 <\/a> <\/div>\n
    \n
    Tubes vides en polypropyl\u00e8ne pour centrifugation de 50 ml, avec bouchons, lot de 50<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n
    \n
    \n Catalog No. 25849 <\/a> <\/div>\n
    \n
    Doses QuEChERS Q-Sep (EN 15662), 4 g MgSO4, 1 g NaCl, 1 g TSCD, 0.5 g DHS, lot de 50 doses<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n
    \n
    \n Catalog No. 26217 <\/a> <\/div>\n
    \n
    Tubes QuEChERS Q-sep pour purification d\u2019extraits par dSPE, 2 ml, pour centrifugation, contenant 150\u00a0mg de MgSO4, 25\u00a0mg de PSA, 2,5\u00a0mg de GCB, lot de 100<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n
    \n
    \n Catalog No. 9314A12 <\/a> <\/div>\n
    \n
    Colonnes Raptor ARC-18, 2,7\u00b5m 100 mm x 2.1 mm DI<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n
    \n
    \n Catalog No. 9314A0252 <\/a> <\/div>\n
    \n
    Cartouche de garde Raptor ARC-18 EXP, 2.7 \u00b5m, L 5\u00a0x DI 2.1 mm, lot de 3<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n
    \n
    \n Catalog No. 9314A62 <\/a> <\/div>\n
    \n
    Colonnes Raptor ARC-18, 2,7\u00b5m 150 x 2.1mm<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n
    \n
    \n Catalog No. 25851 <\/a> <\/div>\n
    \n
    Doses QuEChERS Q-Sep (AOAC 2007.01), 6 g MgSO4, 1.5 g NaOAc, lot de 50 doses<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n
    \n
    \n Catalog No. 25847 <\/a> <\/div>\n
    \n
    Doses QuEChERS Q-Sep (Originale sans tampon), 4 g MgSO4, 1 g NaCl, lot de 50 doses<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n
    \n
    \n Catalog No. 26215 <\/a> <\/div>\n
    \n
    Tube QuEChERS Q-sep pour purification d\u2019extraits par dSPE, 2 ml, pour centrifugation, contenant 150\u00a0mg de MgSO4, 25\u00a0mg de PSA, lot de 100<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n
    \n
    \n Catalog No. 26216 <\/a> <\/div>\n
    \n
    Tubes QuEChERS Q-sep pour purification d\u2019extraits par dSPE, 2 ml, pour centrifugation, contenant 150\u00a0mg de MgSO4, 25\u00a0mg de PSA, 25\u00a0mg de C18-EC, lot de 100<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n
    \n
    \n Catalog No. 26242 <\/a> <\/div>\n
    \n
    Tubes QuEChERS Q-sep pour purification d\u2019extraits par dSPE, 2 ml, pour centrifugation, contenant 150\u00a0mg de MgSO4, 50\u00a0mg de C18-EC, lot de 100<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n <\/div>\n <\/div>\n \n\n\n
    <\/div>\n","protected":false},"excerpt":{"rendered":"

    Dans cette note d\u2019application, nous pr\u00e9sentons une m\u00e9thode simple et efficace pour l\u2019analyse de pesticides, mycotoxines et cannabino\u00efdes dans les bonbons g\u00e9lifi\u00e9s au cannabis. 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