Aumenta l’Efficienza del Laboratorio con un Metodo Consolidato per l’Analisi dei Semivolatili in Tracce

• La rivoluzionaria deattivazione TriMax crea un percorso di flusso del campione robusto ed eccezionalmente inerte per 150 composti, inclusi acidi, basici e neutri.
• La massima inerzia migliora la forma dei picchi per un’ampia gamma di composti semivolatili, consentendo il consolidamento del metodo e una sensibilità a livello di picogrammo.
• Maggiore flessibilità: implementa il nostro metodo per 150 semivolatili oppure ottimizza in pochi secondi le condizioni per il tuo elenco di analiti con il software gratuito EZGC chromatogram modeler di Restek.

L’analisi dei semivolatili rappresenta un’applicazione fondamentale nei laboratori di analisi ambientale di tutto il mondo. Poiché i semivolatili presentano un’ampia variabilità in termini di natura chimica e reattività, vengono spesso analizzati utilizzando colonne diverse; di conseguenza è possibile ottenere significativi incrementi di produttività se i metodi possono essere consolidati su un’unica colonna. Tuttavia, il successo del consolidamento dei metodi dipende dall’efficacia della deattivazione della colonna GC, e le deattivazioni tradizionali tendono a dare buoni risultati per alcune classi di composti ma non per altre. Restek ha sviluppato una tecnologia di deattivazione TriMax di nuova generazione, applicata a tutte le colonne RMX, che ha dimostrato un’efficacia ad ampio spettro, superando anche colonne concorrenti di fascia premium [1].

Uno studio recente ha mostrato che le colonne RMX-5Sil MS producono forme di picco più simmetriche su una gamma più ampia di classi di semivolatili, con il risultato che un numero maggiore di composti soddisfa i requisiti di qualità dei dati in termini di linearità e recupero [2]. La presente applicazione amplia questo lavoro di base ottimizzando le condizioni analitiche ed estendendo l’elenco dei composti target a 150 semivolatili comunemente analizzati, inclusi standard interni e surrogati (Figura 1). Come mostrato in Figura 2, sono stati ottenuti risultati cromatografici eccellenti a livello di tracce (0,1–10 pg on-column) per i semivolatili appartenenti a tutte le classi di composti, inclusi composti acidi reattivi (pentaclorofenolo, 2,4-dinitrofenolo) e composti basici (piridina, benzidina), che spesso sono soggetti a requisiti di qualità dei dati nelle verifiche di idoneità del sistema. Inoltre, la colonna RMX-5Sil MS ha garantito un’adeguata separazione di idrocarburi policiclici aromatici neutri di difficile risoluzione (benzo[b]fluorantene e benzo[k]fluorantene).

Sebbene questo metodo consolidato per l’analisi dei semivolatili in tracce dimostri l’efficacia della colonna RMX-5Sil MS su un ampio elenco di 150 semivolatili comunemente analizzati (n° cat. 31907), i laboratori possono ulteriormente adattarlo alle proprie esigenze utilizzando il software gratuito EZGC chromatogram modeler, che consente di creare istantaneamente metodi ottimizzati per elenchi di analiti specifici e per le dimensioni di colonna preferite.

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Figura 1: Metodo consolidato per l’analisi dei semivolatili in tracce per 150 semivolatili, surrogati e standard interni a 100 ppb (10 pg on-column)

GC_EV1527

Peaks

	Peaks	tR (min)	Conc. (ng/mL)	Mass 1	Product 1	Collision energy 1	Mass 2	Product 2	Collision energy 2
1.	1,4-Dioxane	2.71	10	58	28	6	88	28	14
2.	N-Nitrosodimethylamine	3.02	10	74	44	6	74	42	16
3.	Pyridine	3.08	10	79	52	12	52	26	18
4.	Ethyl methacrylate	3.51	10	69	41	6	99	43	14
5.	2-Picoline	3.91	10	93	66	12	93	65	18
6.	N-Nitrosomethylethylamine	4	10	88	71	6	88	42	16
7.	Methyl methanesulfonate	4.39	10	80	65	8	80	48	28
8.	Acrylamine	4.44	10	71	55	6	71	44	22
9.	2-Fluorophenol	4.62	10	112	92	6	92	63	14
10.	N-Nitrosodiethylamine	4.94	10	102	85	6	102	44	10
11.	Ethyl methanesulfonate	5.38	10	109	45	10	109	79	6
12.	Benzaldehyde	5.88	10	105	77	10	105	51	26
13.	Phenol-d6	6.02	10	99	71	8	71	42	16
14.	Phenol	6.04	10	94	66	10	94	39	30
15.	Aniline	6.07	10	93	66	10	93	65	20
16.	Pentachloroethane	6.14	10	167	132	14	167	95	32
17.	bis-(2-Chloroethyl)ether	6.18	10	93	63	6	63	27	10
18.	2-Chlorophenol	6.25	10	128	64	14	128	63	24
19.	Decane	6.4	10	85	43	6	71	43	6
20.	1,3-Dichlorobenzene	6.51	10	146	111	14	146	75	24
21.	1,4-Dichlorobenzene-d4	6.61	10	150	115	14	150	76	38
22.	1,4-Dichlorobenzene	6.63	10	146	111	14	146	75	24
23.	Benzyl alcohol	6.85	10	108	79	12	108	77	24
24.	1,2-Dichlorobenzene	6.89	10	146	111	12	111	50	36
25.	Indene	7.05	10	115	89	16	116	89	28
26.	2-Methylphenol	7.06	10	108	80	8	108	77	24
27.	2,2′-oxybis(1-chloropropane)	7.11	10	121	45	6	77	51	14
28.	N-Nitrosopyrrolidine	7.28	10	100	43	8	100	55	6
29.	Acetophenone	7.31	10	105	77	12	105	51	26
30.	3- and 4-Methylphenol	7.33	10	70	43	6	107	77	26
31.	N-Nitrosomorpholine	7.331	10	116	86	6	116	56	10
32.	o-Toluidine	7.37	10	106	79	8	107	77	26
33.	Hexachloroethane	7.49	10	201	166	12	201	131	30
34.	Nitrobenzene-d5	7.57	10	128	82	12	82	54	12
35.	Nitrobenzene	7.62	10	123	77	10	123	51	30
36.	N-Nitrosopiperidine	7.88	10	114	84	6	114	97	6
37.	Isophorone	8.05	10	138	82	8	82	54	6
38.	2-Nitrophenol	8.19	10	139	109	8	139	81	12
39.	Benzoic acid	8.31	10	122	77	20	105	77	10
40.	2,4-Dimethylphenol	8.32	10	122	107	12	122	77	26
41.	O,O,O-Triethyl phosphorothioate	8.46	10	121	65	10	198	114	12
42.	Bis(2-chloroethoxy)methane	8.5	10	63	27	12	93	63	6
43.	2,4-Dichlorophenol	8.64	10	98	63	8	162	98	12
44.	Phentermine	8.78	10	58	42	22	134	91	20
45.	1,2,4-Trichlorobenzene	8.8	10	180	145	12	180	109	24
46.	Naphthalene-d8	8.89	10	136	134	14	136	84	20
47.	Naphthalene	8.92	10	128	102	16	129	103	14
48.	α-Terpineol	9	10	136	121	8	136	93	10
49.	4-Chloroaniline	9.06	10	127	100	10	127	65	20
50.	2,6-Dichlorophenol	9.07	10	162	126	8	164	63	26
51.	Hexachloropropene	9.12	10	213	119	18	215	119	18
52.	Hexachlorobutadiene	9.21	10	225	190	14	260	190	26
53.	Quinoline	9.56	10	129	102	16	129	76	26
54.	Caprolactam	9.65	10	113	85	6	113	56	10
55.	1,4-Phenylenediamine	9.73	10	108	81	10	108	80	20
56.	N-Nitrosodibutylamine	9.76	10	116	99	6	116	74	8
57.	4-Chloro-3-methylphenol	10.05	10	142	107	12	142	77	26
58.	Isosafrole I	10.14	10	131	103	8	162	104	12
59.	2-Methylnaphthalene	10.27	10	141	115	16	141	89	30
60.	1-Methylnaphthalene	10.46	10	141	115	16	141	89	30
61.	1,2,4,5-Tetrachlorobenzene	10.61	10	216	181	14	216	108	36
62.	Hexachloropentadiene	10.62	10	272	237	12	237	143	22
63.	2,3-Dichloroaniline	10.83	10	161	90	16	163	90	18
64.	2,4,6-Trichlorophenol	10.85	10	132	97	10	196	97	24
65.	2,4,5-Trichlorophenol	10.95	10	132	97	10	196	97	24
66.	2-Fluorobiphenyl	11.03	10	172	171	12	172	170	22
67.	2-Chloronaphthalene	11.15	10	162	127	16	162	77	30
68.	Isosafrole II	11.17	10	131	103	10	162	104	12
69.	Safrole	11.2	10	162	127	16	131	103	10
70.	Biphenyl	11.21	10	154	152	22	153	126	32
71.	1-Chloronaphthalene	11.25	10	162	127	16	127	77	16
72.	o-Nitroaniline	11.43	10	138	92	12	138	65	22
73.	Diphenyl ether	11.43	10	170	142	10	141	115	14
74.	1,4-Naphthoquinone	11.57	10	158	130	8	158	102	14
75.	1,2-Dinitrobenzene	11.86	10	122	75	12	168	75	20
76.	1,3-Dinitrobenzene	11.87	10	168	75	20	76	50	10
77.	Diphenyl phthalate	11.87	10	163	133	8	163	77	20
78.	1,6-Dinitrotoluene	11.95	10	165	148	8	165	63	20
79.	1,4-Dinitrobenzene	12.01	10	168	51	14	76	63	6
80.	Acenaphthylene	12.02	10	152	126	24	152	76	36
81.	3-Nitroaniline	12.25	10	92	65	8	138	65	20
82.	Acenaphthene-d10	12.32	10	164	162	14	164	160	32
83.	Acenaphthene	12.37	10	153	126	36	153	77	38
84.	2,4-Dinitrophenol	12.46	10	184	154	6	184	107	10
85.	4-Nitrophenol	12.65	10	139	109	6	139	81	14
86.	Pentachlorobenzene	12.66	10	250	215	16	250	142	38
87.	Dibenzofuran	12.73	10	168	139	22	139	63	30
88.	2,4-Dinitrotoluene	12.74	10	165	119	6	165	63	22
89.	1-Naphthylamine	12.88	10	143	116	10	143	115	22
90.	2,3,5,6-Tetrachlorophenol	12.91	10	232	168	12	234	133	26
91.	2,3,4,6-Tetrachlorophenol	13	10	232	168	12	234	131	24
92.	2-Naphthylamine	13.03	10	143	116	10	143	115	22
93.	Diethyl Phthalate	13.3	10	177	149	8	149	65	20
94.	Hexadecane	13.41	10	85	43	6	99	41	14
95.	Fluorene	13.41	10	165	139	26	167	166	14
96.	Zinophos	13.45	10	143	79	10	107	52	20
97.	5-Nitro-o-toluidine	13.45	10	152	106	10	152	77	24
98.	4-Nitroaniline	13.46	10	138	108	8	138	80	18
99.	4-Chlorophenyl phenyl ether	13.46	10	204	77	22	141	115	14
100.	4,6-Dinitro-2-methylphenol	13.54	10	198	168	6	198	121	10
101.	Diphenylamine	13.7	10	169	66	22	169	77	30
102.	Azobenzene	13.76	10	182	105	6	182	77	12
103.	2,4,6-Tribromophenol	13.88	10	330	222	20	332	143	34
104.	Sulfotepp	14.1	10	202	146	10	322	146	24
105.	1,3,5-Trinitrobenzene	14.23	10	213	167	8	213	74	38
106.	Diallate 1	14.31	10	86	43	6	234	150	16
107.	Phorate	14.32	10	75	47	8	121	47	26
108.	Phenacetin	14.35	10	179	137	8	179	109	14
109.	4-Bromophenyl phenyl ether	14.41	10	248	141	14	141	115	12
110.	Diallate 2	14.48	10	234	150	16	86	43	6
111.	Hexachlorobenzene	14.5	10	284	249	14	288	216	26
112.	Dimethoate	14.6	10	93	63	8	125	47	14
113.	Atrazine	14.82	10	200	122	8	215	200	8
114.	Pentachlorophenol	14.9	10	266	167	22	270	169	22
115.	4-Aminobiphenyl	14.93	10	168	141	8	168	167	10
116.	Pentachloronitrobenzene	14.93	10	295	265	8	237	143	20
117.	Propyzamide	15.13	10	173	145	14	254	191	16
118.	Phenanthrene-d10	15.24	10	188	160	20	184	154	32
119.	Octadecane	15.27	10	85	43	6	99	41	14
120.	Phenanthrene	15.29	10	178	152	18	178	151	32
121.	Dinoseb	15.34	10	163	116	14	240	117	24
122.	Disulfoton	15.36	10	88	60	6	97	65	16
123.	Anthracene	15.39	10	178	152	18	178	151	32
124.	Carbazole	15.741	10	167	166	12	167	139	24
125.	Methyl Parathion	16.08	10	263	109	10	263	79	24
126.	di-n-Butyl phthalate	16.58	10	149	121	12	149	65	20
127.	4-Nitroquinoline-N-oxide	16.83	10	190	160	8	101	75	10
128.	Ethyl Parathion	16.89	10	109	81	10	291	81	26
129.	Methapyrilene	17.1	10	97	53	16	190	97	14
130.	Isodrin	17.36	10	261	226	16	261	191	28
131.	Fluoranthene	17.65	10	202	176	26	184	156	18
132.	Fluoranthene	17.65	10	202	152	30	200	174	22
133.	Benzidine	17.99	10	184	166	16	200	149	34
134.	Pyrene	18.08	10	200	150	26	212	208	36
135.	p-Terphenyl-d14	18.5	10	244	242	14	244	240	22
136.	Aramite 1	18.55	10	319	185	6	175	107	14
137.	Aramite 2	18.7	10	185	63	12	319	185	6
138.	p-Dimethylaminoazobenzene	18.79	10	225	148	6	120	77	16
139.	Chlorobenzilate	18.93	10	251	139	12	251	111	30
140.	Famphur	19.4	10	218	109	14	125	79	6
141.	3,3′-Dimethylbenzidine	19.46	10	211	196	8	211	195	16
142.	Kepone	19.47	10	272	237	12	237	143	22
143.	Benzyl butyl phthalate	19.56	10	206	149	8	149	121	10
144.	Bis(2-ethylhexyl) adipate	19.81	10	129	55	14	129	83	8
145.	2-Acetylaminofluorene	19.93	10	223	181	10	181	152	34
146.	Benz[a]anthracene	20.5	10	228	202	22	226	200	28
147.	Chrysene-d12	20.51	10	240	238	14	240	236	30
148.	3,3′-Dichlorobenzidine	20.51	10	252	181	22	252	182	20
149.	4,4′-Methylenebis(2-chloroaniline)	20.53	10	231	195	16	266	231	12
150.	Chrysene	20.56	10	228	202	22	228	201	36
151.	Bis(2-ethylhexyl) phthalate	20.78	10	167	149	8	149	121	14
152.	6-Methylchrysene	21.46	10	242	226	28	239	213	26
153.	Di-n-octyl phthalate	22.08	10	149	121	12	149	93	16
154.	Benzo[b]fluoranthene	22.68	10	252	226	22	250	224	24
155.	7,12-Dimethylbenz[a]anthracene	22.69	10	256	241	12	241	226	14
156.	Benzo[k]fluoranthene	22.74	10	252	226	22	250	224	24
157.	Benzo[a]pyrene	23.41	10	252	226	22	250	224	26
158.	Perylene-d12	23.55	10	264	262	20	264	260	34
159.	3-Methylcholanthrene	24.32	10	268	253	14	252	226	22
160.	Dibenz(a,h)acridine	25.8	10	279	252	34	278	250	24
161.	Dibenz[a,j]acridine	25.88	10	279	277	30	278	250	26
162.	Indeno[1,2,3-cd]pyrene	26.32	10	138	125	12	276	250	30
163.	Dibenz[a,h]anthracene	26.43	10	139	126	8	139	113	14
164.	Benzo[ghi]perylene	27.05	10	138	125	12	138	124	28

Conditions

Column	RMX-5Sil MS, 30 m, 0.25 mm ID, 0.25 µm (cat.# 17323)
Standard/Sample
	SVOC MegaMix 150 kit (cat.# 31907)
	Revised SV internal standard mix (cat.# 31886)
	Base neutral surrogate mix (4/89 SOW) (cat.# 31024)
	Acid surrogate mix (4/89 SOW) (cat.# 31025)
Diluent:	Dichloromethane
Conc.:	100 ppb
Injection
Inj. Vol.:	1 µL split (split ratio 10:1)
Liner:	Topaz 4.0 mm ID Precision liner w/wool (cat.# 23267)
Inj. Temp.:	280 °C
Split Vent Flow Rate:	12 mL/min
Oven
Oven Temp.:	40 °C (hold 1 min) to 280 °C at 12 °C/min to 310 °C at 3 °C/min (hold 1 min)
Carrier Gas	He, constant flow
Flow Rate:	1.2 mL/min @ 40 °C

Detector	SRM/MRM
Source Temp.:	330 °C
Transfer Line Temp.:	280 °C
Analyzer Type:	Triple Quadrupole
Ionization Mode:	EI
Collision Gas:	Ar
Tune Type:	PFTBA
Tune Emission Current:	70 μA
Instrument	Thermo Scientific TSQ 8000 Triple Quadrupole GC-MS
Sample Preparation	Standards were combined and diluted to a concentration of 100 ppb.

Related SKUs

• 31907
• 31886
• 31024
• 31025
• 17323
• 23267

Related Searches

• 8270
• 8270e
• RMX-library
• environmental
• semivolatile
• semivolatiles-gc-library

Download PDF

Figura 2: Le colonne RMX-5Sil MS, altamente inerti, aiutano a soddisfare i requisiti di qualità dei dati per un’ampia gamma di semivolatili complessi a livelli estremamente bassi.

GC_EV1526

Conditions

Column	RMX-5Sil MS, 30 m, 0.25 mm ID, 0.25 µm (cat.# 17323)
Standard/Sample
	SVOC MegaMix 150 kit (cat.# 31907)
	Revised SV internal standard mix (cat.# 31886)
	Base neutral surrogate mix (4/89 SOW) (cat.# 31024)
	Acid surrogate mix (4/89 SOW) (cat.# 31025)
Diluent:	Dichloromethane
Conc.:	1, 10, 100 ppb
Injection
Inj. Vol.:	1 µL split (split ratio 10:1)
Liner:	Topaz 4.0 mm ID Precision liner w/wool (cat.# 23267)
Inj. Temp.:	280 °C
Split Vent Flow Rate:	12 mL/min
Oven
Oven Temp.:	40 °C (hold 1 min) to 280 °C at 12 °C/min to 310 °C at 3 °C/min (hold 1 min)
Carrier Gas	He, constant flow
Flow Rate:	1.2 mL/min @ 40 °C

Detector	SRM/MRM
Source Temp.:	330 °C
Transfer Line Temp.:	280 °C
Analyzer Type:	Triple Quadrupole
Ionization Mode:	EI
Collision Gas:	Ar
Tune Type:	PFTBA
Tune Emission Current:	70 μA
Instrument	Thermo Scientific TSQ 8000 Triple Quadrupole GC-MS

Related SKUs

• 31907
• 31886
• 31024
• 31025
• 17323
• 23267

Related Searches

• RMX-library
• semivolatiles

Download PDF

Bibliografia

1. RMX GC columns brochure, GNBR4923-UNV, Restek Corporation, 2026. https://discover.restek.com/articles/gnbr4923/rmx-gc-columns-unleash-your-performance
2. E. Pack, J. Hoisington, C. English, R. Dhandapani, and C. Myers, Comprehensive trace-level GC-MS/MS semivolatiles method, Application note, EVAN4920-UNV, Restek Corporation, 2025. https://discover.restek.com/it/application-notes-it/evan4920-it/evan4920/metodo-gc-ms-ms-completo-per-i-semivolatili-in-tracce

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Catalog No. 17323

Colonna Capillare GC RMX-5Sil MS, 30 m, 0,25 mm ID, 0,25 µm

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Topaz Inlet Liner Precision, 4,0 mm x 6,3 x 78,5, per GC Thermo TRACE 1300/1310, 1600/1610 con Iniettori SSL, Lana di Quarzo, Deattivazione Premium, 5 pz.

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Leak Detector Elettronico Restek

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Kit SVOC MegaMix 150, 1 mL/ampolla; 6 ampolle/kit

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Miscela di tuning GC-MS, 1000 µg/mL, diclorometano, 1 mL/ampolla

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Miscela di surrogato acido (4/89 SOW), 2000 µg/mL, metanolo, 1 mL/ampolla

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Catalog No. 31024

Miscela di surrogato neutro di base (4/89 SOW), 1000 µg/mL, diclorometano, 1 mL/ampolla

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Catalog No. 31886

Miscela di standard interno SV rivista, 4000 µg/mL, diclorometano, 1 mL/ampolla

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Tags

• Risorse RMX

Authors

• 
  Erica Pack, PhD

  Erica is an interdisciplinary GC applications and technologies scientist at Restek. She obtained her bachelor's degree in forensic biology from The Pennsylvania State University, and her doctorate from Virginia Tech in plant pathology, physiology, and weed science. Since joining Restek in 2021, she has worked with a wide variety of GC columns, including fused silica, MXT, PLOT, and packed columns as well as accessories, such as liners, valves, and methanizers.

  View all posts
• 
  Chris English

  Since 2004, Chris has managed a team of chemists in Restek's innovations laboratory who perform new product testing, method development, and applications work. Before taking the reins of our lab, he spent seven years as an environmental chemist and was critical to the development of Restek’s current line of volatile GC columns. Prior to joining Restek, he operated a variety of gas chromatographic detectors conducting method development and sample analysis. Chris holds a BS in environmental science from Saint Michael's College.

  View all posts
• 
  Ramkumar Dhandapani, PhD

  Dr. Ramkumar Dhandapani is a seasoned analytical chemist with over 23 years of experience in the chromatography industry and a Ph.D. in analytical chemistry. During his career, he has specialized in method development, validation, and the troubleshooting of chromatography methods. He has developed numerous regulatory-compliant methods across diverse sectors, including environmental analysis, food quality and safety, pharmaceutical, fuels, and chemical industries. Currently, Dr. Dhandapani is the Director of Product Management at Restek, he is keen on innovation in chromatography and scaling breakthrough innovations to market as commercial products.

  View all posts
• 
  Colton Myers

  Colton Myers is the R&D manager for sample preparation at Restek Corporation with over 10 years of experience in product development and application innovation, particularly in solid phase microextraction (SPME) and volatile analysis. He has made contributions across various industries, authoring multiple peer-reviewed publications. Starting his career in quality control before transitioning to the GC Innovations team, Colton now leads a team dedicated to advancing sample preparation and collection technologies. He holds a BS in chemistry from Juniata College.

  View all posts

EVFA5253-IT

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