低濃度SVOC分析におけるGC-MSの感度とピーク形状の課題
Key Highlights
- 次世代 TriMax 不活性化処理により、より低い検出限界でも品質基準を満たすデータが取得可能に
- 高い不活性度により、分析が難しい成分を含む多様なSVOCにおいてシャープで対称性の高いピーク形状を実現
- 高感度分析(SIM)と汎用的なスクリーニング(scan)の両方に適したGC-MS分析条件を確立
SVOCのGC-MS分析で検出限界の改善が求められる背景
半揮発性有機化合物の分析を実施するラボでは、顧客要求や溶媒削減(規制対応・コスト削減)のため、検出限界の引き下げが常に求められています。 MS ベースのメソッド(例:EPA 8270)は一般的なアプローチであり、MS を活用することでより低い検出限界を実現できます。
EPA Method 8270に代表されるMSを用いたSVOCの分析手法は広く活用されており、ラボは目的に応じてベストな検出限界を達成できる装置を柔軟に選択できます。例えば、GC-MS/MSのような高感度な装置を採用する場合もある一方で、GC-MSを用いてSIMによる感度向上を図る運用や、より汎用的なscanモードによる分析を選択する場合もあります。
SVOC分析におけるGC-MSのScan法とSIM法の使い分け
SIMとscanはどちらもGC-MSで実施可能ですが、scanが幅広い質量範囲の信号をまとめて取得するシンプルで汎用的な手法であるのに対し、SIMは特定イオンを特定の保持時間に絞って測定することができるため、より高い感度が得られます。SIMはメソッドの設定や維持が煩雑になる傾向がありますが、検出限界の引き下げを検討する場合、新たな装置投資を行わずに感度を高める選択肢として、GC-MSのSIM運用が有力候補になります。
低濃度SVOC分析を想定したGC-MS測定ワークフロー
本研究では、シンプルで堅牢なscanと、GC-MS/MSに代わり得る高感度なSIMという二つのワークフローを目的に応じて選択できるよう、scanとSIMの両モードにおけるGC-MS半揮発性有機化合物分析の条件を確立しました(Figure 1 & Figure 2)。
RMX-5Sil MS カラムによるSVOC分析のクロマトグラフィー性能評価
いずれのメソッドもRMX-5Sil MSカラムを採用しました。このカラムは標準的な5silの選択性を備えながらも、次世代のTriMax不活性化処理により、極めて高い不活性度を実現することが示されています[1,2]。Figure 2に示すように、ベンジジン、ペンタクロロフェノール、2,4-ジニトロフェノールといった主要化合物において、ピーク対称性は一貫して品質目標(≤2)を満たしました。さらに、分離が難しいPAH 類については、EPA 8270のシステム適合性で求められるvalley% 基準(>50%)に対し、benzo[b]fluorantheneと benzo[k]fluorantheneのピーク間 valley% は94%、indeno[1,2,3-cd]pyrene と dibenz[a,h]anthraceneのvalley%は 95%と、極めて良好な結果が得られました。
pgレベルにおけるSVOCの感度とピーク形状の評価結果
また、本稿で示した条件下で RMX-5Sil MS カラムを使用したところ、scan モードでは 1 ng on-column、SIM モードでは 200 pg on-columnという極めて低いオンカラム量においても、幅広い半揮発性有機化合物に対して良好なピーク形状と十分な分離性能が維持され、MSの検出限界近傍においても感度およびクロマトグラフィー性能の両立が可能であることが示されました。
GC-MSによる低濃度SVOC165成分分析の実測データ
GC-MSによる低濃度SVOC 165成分分析におけるRMX-5Sil MSカラムのクロマトグラフィー性能評価のクロマトグラムを以下に示します。
Figure 1. scan Mode (1 ng on-column)
PDFをダウンロードいただくとピークテーブルならびに分析条件をご覧いただけます。
Scanモード:165成分ピークテーブル
| Peak | Compound | tR (min) | Conc. (µg/mL) |
|---|---|---|---|
| 1 | 1,4-Dioxane-d8 | 2.400 | 1 |
| 2 | 1,4-Dioxane | 2.428 | 1 |
| 3 | N-Nitrosodimethylamine | 2.702 | 1 |
| 4 | Pyridine | 2.774 | 1 |
| 5 | Ethyl methacrylate | 3.175 | 1 |
| 6 | 2-Picoline | 3.554 | 1 |
| 7 | N-Nitrosomethylethylamine | 3.648 | 1 |
| 8 | Methyl methanesulfonate | 4.021 | 1 |
| 9 | 2-Fluorophenol | 4.258 | 1 |
| 10 | Acrylamide | 4.543 | 1 |
| 11 | N-Nitrosodiethylamine | 4.875 | 1 |
| 12 | Ethyl methanesulfonate | 4.977 | 1 |
| 13 | Benzaldehyde | 5.454 | 1 |
| 14 | Phenol-d6 | 5.612 | 1 |
| 15 | Phenol | 5.629 | 1 |
| 16 | Aniline | 5.638 | 1 |
| 17 | Pentachloroethane | 5.705 | 1 |
| 18 | Bis(2-chloroethyl)ether | 5.743 | 1 |
| 19 | 2-Chlorophenol | 5.814 | 1 |
| 20 | n-Decane (C10) | 5.962 | 1 |
| 21 | 1,3-Dichlorobenzene | 6.066 | 1 |
| 22 | 1,4-Dichlorobenzene-d4 | 6.153 | 1 |
| 23 | 1,4-Dichlorobenzene | 6.180 | 1 |
| 24 | Benzyl alcohol | 6.393 | 1 |
| 25 | 1,2-Dichlorobenzene | 6.426 | 1 |
| 26 | 2-Methylphenol (o-cresol) | 6.612 | 1 |
| 27 | 2,2′-Oxybis(1-chloropropane) | 6.634 | 1 |
| 28 | N-Nitrosopyrrolidine | 6.765 | 1 |
| 29 | Acetophenone | 6.825 | 1 |
| 30 | N-Nitrosomorpholine | 6.836 | 1 |
| 31 | N-Nitroso-di-n-propylamine | 6.847 | 1 |
| 32 | 3-Methylphenol (m-cresol) | 6.885 | 1 |
| 33 | 4-Methylphenol (p-cresol) | 6.885 | 1 |
| 34 | Indene | 6.885 | 1 |
| 35 | o-Toluidine | 6.890 | 1 |
| 36 | Hexachloroethane | 6.989 | 1 |
| 37 | Nitrobenzene-d5 | 7.067 | 1 |
| 38 | Nitrobenzene | 7.101 | 1 |
| 39 | N-Nitrosopiperidine | 7.347 | 1 |
| 40 | Isophorone | 7.536 | 1 |
| 41 | 2-Nitrophenol | 7.673 | 1 |
| 42 | 2,4-Dimethylphenol | 7.816 | 1 |
| 43 | Benzoic acid | 7.943 | 1 |
| 44 | O,O,O-Triethyl phosphorothioate | 7.943 | 1 |
| 45 | Bis(2-chloroethoxy)methane | 7.970 | 1 |
| 46 | 2,4-Dichlorophenol | 8.113 | 1 |
| 47 | α,α-Dimethylphenethylamine (phentermine) | 8.268 | 1 |
| 48 | 1,2,4-Trichlorobenzene | 8.268 | 1 |
| 49 | Naphthalene-d8 | 8.342 | 1 |
| 50 | Naphthalene | 8.376 | 1 |
| 51 | α-Terpineol | 8.451 | 1 |
| 52 | 4-Chloroaniline | 8.519 | 1 |
| 53 | 2,6-Dichlorophenol | 8.519 | 1 |
| 54 | Hexachloropropene | 8.571 | 1 |
| 55 | Hexachlorobutadiene | 8.674 | 1 |
| Peak | Compound | tR (min) | Conc. (µg/mL) |
|---|---|---|---|
| 56 | Quinoline | 8.988 | 1 |
| 57 | ε-Caprolactam | 9.085 | 1 |
| 58 | 1,4-Phenylenediamine | 9.160 | 1 |
| 59 | N-Nitrosodibutylamine | 9.195 | 1 |
| 60 | 4-Chloro-3-methylphenol | 9.480 | 1 |
| 61 | Isosafrole isomer 2 | 9.560 | 1 |
| 62 | 2-Methylnaphthalene | 9.680 | 1 |
| 63 | 1-Methylnaphthalene | 9.857 | 1 |
| 64 | 1,2,4,5-Tetrachlorobenzene | 10.023 | 1 |
| 65 | Hexachlorocyclopentadiene | 10.023 | 1 |
| 66 | 2,3-Dichloroaniline | 10.217 | 1 |
| 67 | Isosafrole isomer 1 | 10.217 | 1 |
| 68 | 2,4,6-Trichlorophenol | 10.248 | 1 |
| 69 | 2,4,5-Trichlorophenol | 10.303 | 1 |
| 70 | 2-Fluorobiphenyl | 10.412 | 1 |
| 71 | Safrole | 10.547 | 1 |
| 72 | Biphenyl | 10.585 | 1 |
| 73 | 2-Chloronaphthalene | 10.585 | 1 |
| 74 | 1-Chloronaphthalene | 10.623 | 1 |
| 75 | 2-Nitroaniline | 10.801 | 1 |
| 76 | Diphenyl ether | 10.801 | 1 |
| 77 | 1,4-Naphthoquinone | 10.926 | 1 |
| 78 | 1,4-Dinitrobenzene | 11.075 | 1 |
| 79 | Dimethylphthalate | 11.224 | 1 |
| 80 | 1,3-Dinitrobenzene | 11.304 | 1 |
| 81 | 2,6-Dinitrotoluene | 11.304 | 1 |
| 82 | 1,2-Dinitrobenzene | 11.361 | 1 |
| 83 | Acenaphthylene | 11.361 | 1 |
| 84 | 3-Nitroaniline | 11.595 | 1 |
| 85 | Acenaphthene-d10 | 11.647 | 1 |
| 86 | Acenaphthene | 11.704 | 1 |
| 87 | 2,4-Dinitrophenol | 11.809 | 1 |
| 88 | 4-Nitrophenol | 11.996 | 1 |
| 89 | Pentachlorobenzene | 11.996 | 1 |
| 90 | Dibenzofuran | 12.040 | 1 |
| 91 | 2,4-Dinitrotoluene | 12.070 | 1 |
| 92 | 1-Naphthylamine (1-aminonaphthalene) | 12.184 | 1 |
| 93 | 2,3,5,6-Tetrachlorophenol | 12.236 | 1 |
| 94 | 2,3,4,6-Tetrachlorophenol | 12.319 | 1 |
| 95 | 2-Naphthylamine (2-aminonaphthalene) | 12.341 | 1 |
| 96 | Diethylphthalate | 12.602 | 1 |
| 97 | n-Hexadecane (C16) | 12.699 | 1 |
| 98 | Fluorene | 12.699 | 1 |
| 99 | Zalophus (thionazine) | 12.745 | 1 |
| 100 | 4-Chlorophenyl phenyl ether | 12.745 | 1 |
| 101 | 4-Nitroaniline | 12.745 | 1 |
| 102 | 5-Nitro-o-toluidine | 12.745 | 1 |
| 103 | 4,6-Dinitro-2-methylphenol (Dinitro-o-cresol) | 12.853 | 1 |
| 104 | Diphenylamine† | 12.979 | 1 |
| 105 | Azobenzene* | 13.042 | 1 |
| 106 | 2,4,6-Tribromophenol | 13.162 | 1 |
| 107 | Sulfotepp | 13.379 | 1 |
| 108 | 1,3,5-Trinitrobenzene | 13.579 | 1 |
| 109 | Phorate | 13.579 | 1 |
| 110 | Phenacetin | 13.625 | 1 |
| Peak | Compound | tR (min) | Conc. (µg/mL) |
|---|---|---|---|
| 111 | 4-Bromophenyl phenyl ether | 13.677 | 1 |
| 112 | Diallate | 13.734 | 1 |
| 113 | Hexachlorobenzene | 13.785 | 1 |
| 114 | Dimethoate | 13.865 | 1 |
| 115 | Atrazine | 14.071 | 1 |
| 116 | 4-Aminobiphenyl | 14.168 | 1 |
| 117 | Pentachlorophenol | 14.170 | 1 |
| 118 | Pentachloronitrobenzene (Quintozene) | 14.214 | 1 |
| 119 | Propyzamide | 14.380 | 1 |
| 120 | Phenanthrene-d10 | 14.477 | 1 |
| 121 | n-Octadecane (C18) | 14.517 | 1 |
| 122 | Phenanthrene | 14.517 | 1 |
| 123 | Dinoseb | 14.599 | 1 |
| 124 | Disulfoton | 14.599 | 1 |
| 125 | Anthracene | 14.614 | 1 |
| 126 | Carbazole | 14.963 | 1 |
| 127 | Methyl parathion | 15.295 | 1 |
| 128 | Di-n-butyl phthalate | 15.775 | 1 |
| 129 | 4-Nitroquinoline-N-oxide | 16.027 | 1 |
| 130 | Parathion (ethyl parathion) | 16.078 | 1 |
| 131 | Methapyrilene hydrochloride | 16.273 | 1 |
| 132 | Isodrin | 16.518 | 1 |
| 133 | Fluoranthene | 16.804 | 1 |
| 134 | Benzidine | 17.127 | 1 |
| 135 | Pyrene | 17.222 | 1 |
| 136 | p-Terphenyl-d14 | 17.622 | 1 |
| 137 | Aramite isomer 2 | 17.668 | 1 |
| 138 | Aramite isomer 1 | 17.822 | 1 |
| 139 | p-Dimethylaminoazobenzene | 17.908 | 1 |
| 140 | Chlorobenzilate | 18.034 | 1 |
| 141 | Famphur | 18.485 | 1 |
| 142 | 3,3′-Dimethylbenzidine (o-tolidine) | 18.548 | 1 |
| 143 | Kepone | 18.548 | 1 |
| 144 | Benzyl butyl phthalate | 18.640 | 1 |
| 145 | Bis(2-ethylhexyl)adipate | 18.891 | 1 |
| 146 | 2-Acetylaminofluorene | 19.017 | 1 |
| 147 | 4,4′-Methylene-bis(2-chloroaniline) | 19.108 | 1 |
| 148 | 3,3′-Dichlorobenzidine | 19.560 | 1 |
| 149 | Benz[a]anthracene | 19.560 | 1 |
| 150 | Chrysene-d12 | 19.560 | 1 |
| 151 | Chrysene | 19.612 | 1 |
| 152 | Bis(2-ethylhexyl)phthalate | 19.823 | 1 |
| 153 | 6-Methylchrysene | 20.475 | 1 |
| 154 | Di-n-octyl phthalate | 21.030 | 1 |
| 155 | Benzo[b]fluoranthene | 21.590 | 1 |
| 156 | 7,12-Dimethylbenz[a]anthracene | 21.590 | 1 |
| 157 | Benzo[k]fluoranthene | 21.641 | 1 |
| 158 | Benzo[a]pyrene | 22.248 | 1 |
| 159 | Perylene-d12 | 22.379 | 1 |
| 160 | 3-Methylcholanthrene | 23.082 | 1 |
| 161 | Dibenz(a,h)acridine | 24.357 | 1 |
| 162 | Dibenz[a,j]acridine | 24.483 | 1 |
| 163 | Indeno[1,2,3-cd]pyrene | 24.883 | 1 |
| 164 | Dibenz[a,h]anthracene | 24.969 | 1 |
| 165 | Benzo[g,h,i]perylene | 25.541 | 1 |
Figure 2. SIM Mode (200 pg on-column)
PDFをダウンロードいただくとピークテーブルならびに分析条件をご覧いただけます。
SIMモード:165成分のピークテーブル
| Peak | Compound | tR (min) | Conc. (ng/mL) |
SIM Ion | Dwell (ms) |
Ion Group |
|---|---|---|---|---|---|---|
| 1 | 1,4-Dioxane-d8 | 2.401 | 200 | 96 | 25 | 1 |
| 2 | 1,4-Dioxane | 2.427 | 200 | 88 | 25 | 1 |
| 3 | N-Nitrosodimethylamine | 2.702 | 200 | 74 | 25 | 1 |
| 4 | Pyridine | 2.774 | 200 | 79 | 25 | 1 |
| 5 | Ethyl methacrylate | 3.175 | 200 | 69 | 25 | 1 |
| 6 | 2-Picoline | 3.554 | 200 | 93 | 25 | 1 |
| 7 | N-Nitrosomethylethylamine | 3.648 | 200 | 42 | 25 | 1 |
| 8 | Methyl methanesulfonate | 4.021 | 200 | 80 | 25 | 1 |
| 9 | 2-Fluorophenol | 4.258 | 200 | 112 | 25 | 1 |
| 10 | Acrylamide | 4.543 | 200 | 71 | 25 | 1 |
| 11 | N-Nitrosodiethylamine | 4.977 | 200 | 102 | 25 | 1 |
| 12 | Ethyl methanesulfonate | 4.977 | 200 | 109 | 25 | 1 |
| 13 | Benzaldehyde | 5.454 | 200 | 77 | 11 | 2 |
| 14 | Phenol-d6 | 5.612 | 200 | 99 | 11 | 2 |
| 15 | Phenol | 5.633 | 200 | 94 | 11 | 2 |
| 16 | Aniline | 5.633 | 200 | 93 | 11 | 2 |
| 17 | Pentachloroethane | 5.7 | 200 | 167 | 11 | 2 |
| 18 | Bis(2-chloroethyl)ether | 5.743 | 200 | 63 | 11 | 2 |
| 19 | 2-Chlorophenol | 5.814 | 200 | 128 | 11 | 2 |
| 20 | n-Decane (C10) | 5.962 | 200 | 57 | 11 | 2 |
| 21 | 1,3-Dichlorobenzene | 6.066 | 200 | 146 | 11 | 2 |
| 22 | 1,4-Dichlorobenzene-d4 | 6.154 | 200 | 150 | 11 | 2 |
| 23 | 1,4-Dichlorobenzene | 6.18 | 200 | 148 | 11 | 2 |
| 24 | Benzyl alcohol | 6.393 | 200 | 79 | 11 | 2 |
| 25 | 1,2-Dichlorobenzene | 6.426 | 200 | 111 | 11 | 2 |
| 26 | 2-Methylphenol (o-cresol) | 6.611 | 200 | 108 | 11 | 2 |
| 27 | 2,2′-Oxybis(1-chloropropane) | 6.634 | 200 | 45 | 11 | 2 |
| 28 | N-Nitrosopyrrolidine | 6.765 | 200 | 100 | 11 | 2 |
| 29 | Acetophenone | 6.825 | 200 | 105 | 11 | 2 |
| 30 | N-Nitrosomorpholine | 6.825 | 200 | 56 | 11 | 2 |
| 31 | N-Nitroso-di-n-propylamine | 6.825 | 200 | 43 | 11 | 2 |
| 32 | 3-Methylphenol (m-cresol) | 6.885 | 200 | 80 | 11 | 2 |
| 33 | 4-Methylphenol (p-cresol) | 6.885 | 200 | 107 | 11 | 2 |
| 34 | Indene | 6.885 | 200 | 117 | 11 | 2 |
| 35 | o-Toluidine | 6.885 | 200 | 106 | 11 | 2 |
| 36 | Hexachloroethane | 6.989 | 200 | 119 | 11 | 2 |
| 37 | Nitrobenzene-d5 | 7.068 | 200 | 82 | 11 | 2 |
| 38 | Nitrobenzene | 7.1 | 200 | 123 | 11 | 2 |
| 39 | N-Nitrosopiperidine | 7.347 | 200 | 114 | 17 | 3 |
| 40 | Isophorone | 7.531 | 200 | 82 | 17 | 3 |
| 41 | 2-Nitrophenol | 7.671 | 200 | 139 | 17 | 3 |
| 42 | 2,4-Dimethylphenol | 7.811 | 200 | 122 | 17 | 3 |
| 43 | Benzoic acid | 7.898 | 200 | 105 | 17 | 3 |
| 44 | O,O,O-Triethyl phosphorothioate | 7.942 | 200 | 121 | 17 | 3 |
| 45 | Bis(2-chloroethoxy)methane | 7.969 | 200 | 93 | 17 | 3 |
| 46 | 2,4-Dichlorophenol | 8.113 | 200 | 162 | 17 | 3 |
| 47 | α,α-Dimethylphenethylamine (phentermine) | 8.178 | 200 | 58 | 17 | 3 |
| 48 | 1,2,4-Trichlorobenzene | 8.264 | 200 | 180 | 17 | 3 |
| 49 | Naphthalene-d8 | 8.34 | 200 | 136 | 17 | 3 |
| 50 | Naphthalene | 8.378 | 200 | 128 | 17 | 3 |
| 51 | α-Terpineol | 8.453 | 200 | 59 | 17 | 3 |
| 52 | 4-Chloroaniline | 8.518 | 200 | 127 | 17 | 3 |
| 53 | 2,6-Dichlorophenol | 8.518 | 200 | 164 | 17 | 3 |
| 54 | Hexachloropropene | 8.572 | 200 | 213 | 17 | 3 |
| 55 | Hexachlorobutadiene | 8.674 | 200 | 225 | 17 | 3 |
| 56 | Quinoline | 8.993 | 200 | 129 | 15 | 4 |
| 57 | ε-Caprolactam | 9.085 | 200 | 55 | 15 | 4 |
| 58 | 1,4-Phenylenediamine | 9.160 | 200 | 108 | 15 | 4 |
| 59 | N-Nitrosodibutylamine | 9.195 | 200 | 84 | 15 | 4 |
| 60 | 4-Chloro-3-methylphenol | 9.477 | 200 | 107 | 15 | 4 |
| 61 | Isosafrole isomer 2 | 9.563 | 200 | 181 | 15 | 4 |
| 62 | 2-Methylnaphthalene | 9.681 | 200 | 142 | 15 | 4 |
| 63 | 1-Methylnaphthalene | 9.858 | 200 | 141 | 15 | 4 |
| 64 | 1,2,4,5-Tetrachlorobenzene | 10.024 | 200 | 216 | 15 | 4 |
| 65 | Hexachlorocyclopentadiene | 10.024 | 200 | 237 | 15 | 4 |
| 66 | 2,3-Dichloroaniline | 10.221 | 200 | 161 | 15 | 4 |
| 67 | Isosafrole isomer 1 | 10.221 | 200 | 104 | 15 | 4 |
| 68 | 2,4,6-Trichlorophenol | 10.25 | 200 | 196 | 15 | 4 |
| 69 | 2,4,5-Trichlorophenol | 10.303 | 200 | 198 | 15 | 4 |
| 70 | 2-Fluorobiphenyl | 10.41 | 200 | 172 | 15 | 4 |
| 71 | Safrole | 10.549 | 200 | 131 | 15 | 4 |
| 72 | Biphenyl | 10.586 | 200 | 154 | 15 | 4 |
| 73 | 2-Chloronaphthalene | 10.586 | 200 | 162 | 15 | 5 |
| 74 | 1-Chloronaphthalene | 10.624 | 200 | 127 | 15 | 5 |
| 75 | 2-Nitroaniline | 10.803 | 200 | 138 | 13 | 5 |
| 76 | Diphenyl ether | 10.803 | 200 | 170 | 15 | 5 |
| 77 | 1,4-Naphthoquinone | 10.927 | 200 | 158 | 13 | 5 |
| 78 | 1,4-Dinitrobenzene | 11.073 | 200 | 168 | 13 | 5 |
| 79 | Dimethylphthalate | 11.223 | 200 | 163 | 13 | 5 |
| 80 | 1,3-Dinitrobenzene | 11.301 | 200 | 76 | 13 | 5 |
| 81 | 2,6-Dinitrotoluene | 11.301 | 200 | 165 | 13 | 5 |
| 82 | 1,2-Dinitrobenzene | 11.363 | 200 | 50 | 13 | 5 |
| Peak | Compound | tR (min) | Conc. (ng/mL) |
SIM Ion | Dwell (ms) |
Ion Group |
|---|---|---|---|---|---|---|
| 83 | Acenaphthylene | 11.363 | 200 | 152 | 13 | 5 |
| 84 | 3-Nitroaniline | 11.591 | 200 | 65 | 13 | 5 |
| 85 | Acenaphthene-d10 | 11.649 | 200 | 162 | 13 | 5 |
| 86 | Acenaphthene | 11.706 | 200 | 153 | 13 | 5 |
| 87 | 2,4-Dinitrophenol | 11.809 | 200 | 184 | 13 | 5 |
| 88 | 4-Nitrophenol | 11.996 | 200 | 139 | 13 | 5 |
| 89 | Pentachlorobenzene | 11.996 | 200 | 250 | 13 | 5 |
| 90 | Dibenzofuran | 12.043 | 200 | 84 | 13 | 5 |
| 91 | 2,4-Dinitrotoluene | 12.183 | 200 | 89 | 13 | 5 |
| 92 | 1-Naphthylamine (1-aminonaphthalene) | 12.235 | 200 | 143 | 13 | 5 |
| 93 | 2,3,5,6-Tetrachlorophenol | 12.339 | 200 | 232 | 13 | 5 |
| 94 | 2,3,4,6-Tetrachlorophenol | 12.339 | 200 | 230 | 13 | 5 |
| 95 | 2-Naphthylamine (2-aminonaphthalene) | 12.339 | 200 | 115 | 13 | 5 |
| 96 | Diethylphthalate | 12.596 | 200 | 149 | 13 | 5 |
| 97 | n-Hexadecane (C16) | 12.703 | 200 | 57 | 29 | 6 |
| 98 | Fluorene | 12.703 | 200 | 166 | 29 | 6 |
| 99 | Zalophus (thionazine) | 12.746 | 200 | 107 | 29 | 6 |
| 100 | 4-Chlorophenyl phenyl ether | 12.746 | 200 | 204 | 29 | 6 |
| 101 | 4-Nitroaniline | 12.746 | 200 | 65 | 29 | 6 |
| 102 | 5-Nitro-o-toluidine | 12.746 | 200 | 152 | 29 | 6 |
| 103 | 4,6-Dinitro-2-methylphenol (Dinitro-o-cresol) | 12.852 | 200 | 198 | 29 | 6 |
| 104 | Diphenylamine† | 12.98 | 200 | 169 | 29 | 6 |
| 105 | Azobenzene* | 13.044 | 200 | 77 | 29 | 6 |
| 106 | 2,4,6-Tribromophenol | 13.162 | 200 | 330 | 29 | 6 |
| 107 | Sulfotepp | 13.385 | 200 | 322 | 14 | 7 |
| 108 | 1,3,5-Trinitrobenzene | 13.581 | 200 | 213 | 14 | 7 |
| 109 | Phenacetin | 13.581 | 200 | 108 | 14 | 7 |
| 110 | Phorate | 13.618 | 200 | 75 | 14 | 7 |
| 111 | 4-Bromophenyl phenyl ether | 13.677 | 200 | 248 | 14 | 7 |
| 112 | Diallate | 13.735 | 200 | 43 | 14 | 7 |
| 113 | Hexachlorobenzene | 13.788 | 200 | 284 | 14 | 7 |
| 114 | Dimethoate | 13.857 | 200 | 87 | 14 | 7 |
| 115 | Atrazine | 14.064 | 200 | 200 | 14 | 7 |
| 116 | 4-Aminobiphenyl | 14.17 | 200 | 169 | 14 | 7 |
| 117 | Pentachlorophenol | 14.17 | 200 | 266 | 14 | 7 |
| 118 | Pentachloronitrobenzene (Quintozene) | 14.213 | 200 | 237 | 14 | 7 |
| 119 | Propyzamide | 14.377 | 200 | 173 | 14 | 7 |
| 120 | Phenanthrene-d10 | 14.477 | 200 | 188 | 14 | 7 |
| 121 | n-Octadecane (C18) | 14.52 | 200 | 57 | 14 | 7 |
| 122 | Phenanthrene | 14.52 | 200 | 178 | 14 | 7 |
| 123 | Dinoseb | 14.616 | 200 | 211 | 14 | 7 |
| 124 | Disulfoton | 14.616 | 200 | 88 | 14 | 7 |
| 125 | Anthracene | 14.616 | 200 | 179 | 14 | 7 |
| 126 | Carbazole | 14.961 | 200 | 167 | 30 | 8 |
| 127 | Methyl parathion | 15.296 | 200 | 109 | 30 | 8 |
| 128 | Di-n-butyl phthalate | 15.779 | 200 | 149 | 30 | 8 |
| 129 | 4-Nitroquinoline-N-oxide | 16.026 | 200 | 190 | 30 | 8 |
| 130 | Parathion (ethyl parathion) | 16.075 | 200 | 291 | 30 | 8 |
| 131 | Methapyrilene hydrochloride | 16.273 | 200 | 58 | 30 | 8 |
| 132 | Isodrin | 16.52 | 200 | 193 | 30 | 8 |
| 133 | Fluoranthene | 16.806 | 200 | 202 | 30 | 8 |
| 134 | Benzidine | 17.124 | 200 | 184 | 30 | 8 |
| 135 | Pyrene | 17.223 | 200 | 203 | 30 | 8 |
| 136 | p-Terphenyl-d14 | 17.627 | 200 | 244 | 27 | 9 |
| 137 | Aramite isomer 2 | 17.627 | 200 | 175 | 27 | 9 |
| 138 | Aramite isomer 1 | 17.818 | 200 | 135 | 27 | 9 |
| 139 | p-Dimethylaminoazobenzene | 17.905 | 200 | 120 | 27 | 9 |
| 140 | Chlorobenzilate | 18.041 | 200 | 251 | 27 | 9 |
| 141 | Famphur | 18.487 | 200 | 218 | 27 | 9 |
| 142 | 3,3′-Dimethylbenzidine (o-tolidine) | 18.553 | 200 | 254 | 15 | 9 |
| 143 | Kepone | 18.553 | 200 | 272 | 27 | 9 |
| 144 | Benzyl butyl phthalate | 18.64 | 200 | 149 | 27 | 9 |
| 145 | Bis(2-ethylhexyl)adipate | 18.89 | 200 | 129 | 27 | 9 |
| 146 | 2-Acetylaminofluorene | 19.015 | 200 | 181 | 27 | 9 |
| 147 | 4,4′-Methylene-bis(2-chloroaniline) | 19.561 | 200 | 231 | 15 | 9 |
| 148 | 3,3′-Dichlorobenzidine | 19.561 | 200 | 212 | 27 | 9 |
| 149 | Benz[a]anthracene | 19.561 | 200 | 228 | 15 | 10 |
| 150 | Chrysene-d12 | 19.561 | 200 | 240 | 15 | 10 |
| 151 | Chrysene | 19.61 | 200 | 226 | 15 | 10 |
| 152 | Bis(2-ethylhexyl)phthalate | 19.824 | 200 | 167 | 15 | 10 |
| 153 | 6-Methylchrysene | 20.473 | 200 | 242 | 15 | 10 |
| 154 | Di-n-octyl phthalate | 21.031 | 200 | 149 | 15 | 10 |
| 155 | Benzo[b]fluoranthene | 21.589 | 200 | 57 | 15 | 10 |
| 156 | 7,12-Dimethylbenz[a]anthracene | 21.589 | 200 | 256 | 15 | 10 |
| 157 | Benzo[k]fluoranthene | 21.637 | 200 | 252 | 15 | 10 |
| 158 | Benzo[a]pyrene | 22.249 | 200 | 253 | 15 | 10 |
| 159 | Perylene-d12 | 22.377 | 200 | 264 | 15 | 10 |
| 160 | 3-Methylcholanthrene | 23.08 | 200 | 268 | 15 | 10 |
| 161 | Dibenz(a,h)acridine | 24.357 | 200 | 279 | 15 | 10 |
| 162 | Dibenz[a,j]acridine | 24.48 | 200 | 280 | 15 | 10 |
| 163 | Indeno[1,2,3-cd]pyrene | 24.882 | 200 | 277 | 15 | 10 |
| 164 | Dibenz[a,h]anthracene | 24.968 | 200 | 278 | 15 | 10 |
| 165 | Benzo[g,h,i]perylene | 25.537 | 200 | 276 | 15 | 10 |
まとめ:低濃度SVOCのGC-MS分析で感度とピーク形状を両立するために
低濃度の半揮発性有機化合物(SVOC)をGC-MSで分析する際には、感度低下やピーク形状の劣化が大きな課題となります。本記事で示した結果から、カラムの不活性度を含むシステム全体の最適化により、scanおよびSIMのいずれにおいても高品質な分析が可能であることが示されました。
References 参照文献
- E. Pack, J. Hoisington, C. English, R. Dhandapani, and C. Myers, 微量レベル半揮発性有機化合物のGC-MS/MS一斉分析法:データ品質の維持と検出下限の改善, Application note, EVAN4920-JA, Restek Corporation, 2025.
- RMX GCカラムカタログ, GNBR4923A-JA, Restek Corporation, 2026.







