技術資料

GC-MS半揮発性有機化合物分析:微量分析の限界に挑む

19 Jan 2026

薬物, GCカラム, 分析条件, クロマトグラム

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。

お問い合わせ|Restek

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。

Semivolatiles on RMX-5Sil MS by Method 8270D (GC-MS in Scan Mode)

GC_GN1250

Scanモード:165成分ピークテーブル

Peak Compound tR (min) Conc.
(µg/mL)
11,4-Dioxane-d82.4001
21,4-Dioxane2.4281
3N-Nitrosodimethylamine2.7021
4Pyridine2.7741
5Ethyl methacrylate3.1751
62-Picoline3.5541
7N-Nitrosomethylethylamine3.6481
8Methyl methanesulfonate4.0211
92-Fluorophenol4.2581
10Acrylamide4.5431
11N-Nitrosodiethylamine4.8751
12Ethyl methanesulfonate4.9771
13Benzaldehyde5.4541
14Phenol-d65.6121
15Phenol5.6291
16Aniline5.6381
17Pentachloroethane5.7051
18Bis(2-chloroethyl)ether5.7431
192-Chlorophenol5.8141
20n-Decane (C10)5.9621
211,3-Dichlorobenzene6.0661
221,4-Dichlorobenzene-d46.1531
231,4-Dichlorobenzene6.1801
24Benzyl alcohol6.3931
251,2-Dichlorobenzene6.4261
262-Methylphenol (o-cresol)6.6121
272,2′-Oxybis(1-chloropropane)6.6341
28N-Nitrosopyrrolidine6.7651
29Acetophenone6.8251
30N-Nitrosomorpholine6.8361
31N-Nitroso-di-n-propylamine6.8471
323-Methylphenol (m-cresol)6.8851
334-Methylphenol (p-cresol)6.8851
34Indene6.8851
35o-Toluidine6.8901
36Hexachloroethane6.9891
37Nitrobenzene-d57.0671
38Nitrobenzene7.1011
39N-Nitrosopiperidine7.3471
40Isophorone7.5361
412-Nitrophenol7.6731
422,4-Dimethylphenol7.8161
43Benzoic acid7.9431
44O,O,O-Triethyl phosphorothioate7.9431
45Bis(2-chloroethoxy)methane7.9701
462,4-Dichlorophenol8.1131
47α,α-Dimethylphenethylamine (phentermine)8.2681
481,2,4-Trichlorobenzene8.2681
49Naphthalene-d88.3421
50Naphthalene8.3761
51α-Terpineol8.4511
524-Chloroaniline8.5191
532,6-Dichlorophenol8.5191
54Hexachloropropene8.5711
55Hexachlorobutadiene8.6741
Peak Compound tR (min) Conc.
(µg/mL)
56Quinoline8.9881
57ε-Caprolactam9.0851
581,4-Phenylenediamine9.1601
59N-Nitrosodibutylamine9.1951
604-Chloro-3-methylphenol9.4801
61Isosafrole isomer 29.5601
622-Methylnaphthalene9.6801
631-Methylnaphthalene9.8571
641,2,4,5-Tetrachlorobenzene10.0231
65Hexachlorocyclopentadiene10.0231
662,3-Dichloroaniline10.2171
67Isosafrole isomer 110.2171
682,4,6-Trichlorophenol10.2481
692,4,5-Trichlorophenol10.3031
702-Fluorobiphenyl10.4121
71Safrole10.5471
72Biphenyl10.5851
732-Chloronaphthalene10.5851
741-Chloronaphthalene10.6231
752-Nitroaniline10.8011
76Diphenyl ether10.8011
771,4-Naphthoquinone10.9261
781,4-Dinitrobenzene11.0751
79Dimethylphthalate11.2241
801,3-Dinitrobenzene11.3041
812,6-Dinitrotoluene11.3041
821,2-Dinitrobenzene11.3611
83Acenaphthylene11.3611
843-Nitroaniline11.5951
85Acenaphthene-d1011.6471
86Acenaphthene11.7041
872,4-Dinitrophenol11.8091
884-Nitrophenol11.9961
89Pentachlorobenzene11.9961
90Dibenzofuran12.0401
912,4-Dinitrotoluene12.0701
921-Naphthylamine (1-aminonaphthalene)12.1841
932,3,5,6-Tetrachlorophenol12.2361
942,3,4,6-Tetrachlorophenol12.3191
952-Naphthylamine (2-aminonaphthalene)12.3411
96Diethylphthalate12.6021
97n-Hexadecane (C16)12.6991
98Fluorene12.6991
99Zalophus (thionazine)12.7451
1004-Chlorophenyl phenyl ether12.7451
1014-Nitroaniline12.7451
1025-Nitro-o-toluidine12.7451
1034,6-Dinitro-2-methylphenol (Dinitro-o-cresol)12.8531
104Diphenylamine†12.9791
105Azobenzene*13.0421
1062,4,6-Tribromophenol13.1621
107Sulfotepp13.3791
1081,3,5-Trinitrobenzene13.5791
109Phorate13.5791
110Phenacetin13.6251
Peak Compound tR (min) Conc.
(µg/mL)
1114-Bromophenyl phenyl ether13.6771
112Diallate13.7341
113Hexachlorobenzene13.7851
114Dimethoate13.8651
115Atrazine14.0711
1164-Aminobiphenyl14.1681
117Pentachlorophenol14.1701
118Pentachloronitrobenzene (Quintozene)14.2141
119Propyzamide14.3801
120Phenanthrene-d1014.4771
121n-Octadecane (C18)14.5171
122Phenanthrene14.5171
123Dinoseb14.5991
124Disulfoton14.5991
125Anthracene14.6141
126Carbazole14.9631
127Methyl parathion15.2951
128Di-n-butyl phthalate15.7751
1294-Nitroquinoline-N-oxide16.0271
130Parathion (ethyl parathion)16.0781
131Methapyrilene hydrochloride16.2731
132Isodrin16.5181
133Fluoranthene16.8041
134Benzidine17.1271
135Pyrene17.2221
136p-Terphenyl-d1417.6221
137Aramite isomer 217.6681
138Aramite isomer 117.8221
139p-Dimethylaminoazobenzene17.9081
140Chlorobenzilate18.0341
141Famphur18.4851
1423,3′-Dimethylbenzidine (o-tolidine)18.5481
143Kepone18.5481
144Benzyl butyl phthalate18.6401
145Bis(2-ethylhexyl)adipate18.8911
1462-Acetylaminofluorene19.0171
1474,4′-Methylene-bis(2-chloroaniline)19.1081
1483,3′-Dichlorobenzidine19.5601
149Benz[a]anthracene19.5601
150Chrysene-d1219.5601
151Chrysene19.6121
152Bis(2-ethylhexyl)phthalate19.8231
1536-Methylchrysene20.4751
154Di-n-octyl phthalate21.0301
155Benzo[b]fluoranthene21.5901
1567,12-Dimethylbenz[a]anthracene21.5901
157Benzo[k]fluoranthene21.6411
158Benzo[a]pyrene22.2481
159Perylene-d1222.3791
1603-Methylcholanthrene23.0821
161Dibenz(a,h)acridine24.3571
162Dibenz[a,j]acridine24.4831
163Indeno[1,2,3-cd]pyrene24.8831
164Dibenz[a,h]anthracene24.9691
165Benzo[g,h,i]perylene25.5411
RMX Graphic Ad EZGC HTML Block Mock UpーJP 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。

Semivolatiles on RMX-5Sil MS by 8270D (GC-MS in SIM Mode)

GC_GN1251

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
11,4-Dioxane-d82.40120096251
21,4-Dioxane2.42720088251
3N-Nitrosodimethylamine2.70220074251
4Pyridine2.77420079251
5Ethyl methacrylate3.17520069251
62-Picoline3.55420093251
7N-Nitrosomethylethylamine3.64820042251
8Methyl methanesulfonate4.02120080251
92-Fluorophenol4.258200112251
10Acrylamide4.54320071251
11N-Nitrosodiethylamine4.977200102251
12Ethyl methanesulfonate4.977200109251
13Benzaldehyde5.45420077112
14Phenol-d65.61220099112
15Phenol5.63320094112
16Aniline5.63320093112
17Pentachloroethane5.7200167112
18Bis(2-chloroethyl)ether5.74320063112
192-Chlorophenol5.814200128112
20n-Decane (C10)5.96220057112
211,3-Dichlorobenzene6.066200146112
221,4-Dichlorobenzene-d46.154200150112
231,4-Dichlorobenzene6.18200148112
24Benzyl alcohol6.39320079112
251,2-Dichlorobenzene6.426200111112
262-Methylphenol (o-cresol)6.611200108112
272,2′-Oxybis(1-chloropropane)6.63420045112
28N-Nitrosopyrrolidine6.765200100112
29Acetophenone6.825200105112
30N-Nitrosomorpholine6.82520056112
31N-Nitroso-di-n-propylamine6.82520043112
323-Methylphenol (m-cresol)6.88520080112
334-Methylphenol (p-cresol)6.885200107112
34Indene6.885200117112
35o-Toluidine6.885200106112
36Hexachloroethane6.989200119112
37Nitrobenzene-d57.06820082112
38Nitrobenzene7.1200123112
39N-Nitrosopiperidine7.347200114173
40Isophorone7.53120082173
412-Nitrophenol7.671200139173
422,4-Dimethylphenol7.811200122173
43Benzoic acid7.898200105173
44O,O,O-Triethyl phosphorothioate7.942200121173
45Bis(2-chloroethoxy)methane7.96920093173
462,4-Dichlorophenol8.113200162173
47α,α-Dimethylphenethylamine (phentermine)8.17820058173
481,2,4-Trichlorobenzene8.264200180173
49Naphthalene-d88.34200136173
50Naphthalene8.378200128173
51α-Terpineol8.45320059173
524-Chloroaniline8.518200127173
532,6-Dichlorophenol8.518200164173
54Hexachloropropene8.572200213173
55Hexachlorobutadiene8.674200225173
56Quinoline8.993200129154
57ε-Caprolactam9.08520055154
581,4-Phenylenediamine9.160200108154
59N-Nitrosodibutylamine9.19520084154
604-Chloro-3-methylphenol9.477200107154
61Isosafrole isomer 29.563200181154
622-Methylnaphthalene9.681200142154
631-Methylnaphthalene9.858200141154
641,2,4,5-Tetrachlorobenzene10.024200216154
65Hexachlorocyclopentadiene10.024200237154
662,3-Dichloroaniline10.221200161154
67Isosafrole isomer 110.221200104154
682,4,6-Trichlorophenol10.25200196154
692,4,5-Trichlorophenol10.303200198154
702-Fluorobiphenyl10.41200172154
71Safrole10.549200131154
72Biphenyl10.586200154154
732-Chloronaphthalene10.586200162155
741-Chloronaphthalene10.624200127155
752-Nitroaniline10.803200138135
76Diphenyl ether10.803200170155
771,4-Naphthoquinone10.927200158135
781,4-Dinitrobenzene11.073200168135
79Dimethylphthalate11.223200163135
801,3-Dinitrobenzene11.30120076135
812,6-Dinitrotoluene11.301200165135
821,2-Dinitrobenzene11.36320050135
Peak Compound tR (min) Conc.
(ng/mL)
SIM Ion Dwell
(ms)
Ion
Group
83Acenaphthylene11.363200152135
843-Nitroaniline11.59120065135
85Acenaphthene-d1011.649200162135
86Acenaphthene11.706200153135
872,4-Dinitrophenol11.809200184135
884-Nitrophenol11.996200139135
89Pentachlorobenzene11.996200250135
90Dibenzofuran12.04320084135
912,4-Dinitrotoluene12.18320089135
921-Naphthylamine (1-aminonaphthalene)12.235200143135
932,3,5,6-Tetrachlorophenol12.339200232135
942,3,4,6-Tetrachlorophenol12.339200230135
952-Naphthylamine (2-aminonaphthalene)12.339200115135
96Diethylphthalate12.596200149135
97n-Hexadecane (C16)12.70320057296
98Fluorene12.703200166296
99Zalophus (thionazine)12.746200107296
1004-Chlorophenyl phenyl ether12.746200204296
1014-Nitroaniline12.74620065296
1025-Nitro-o-toluidine12.746200152296
1034,6-Dinitro-2-methylphenol (Dinitro-o-cresol)12.852200198296
104Diphenylamine†12.98200169296
105Azobenzene*13.04420077296
1062,4,6-Tribromophenol13.162200330296
107Sulfotepp13.385200322147
1081,3,5-Trinitrobenzene13.581200213147
109Phenacetin13.581200108147
110Phorate13.61820075147
1114-Bromophenyl phenyl ether13.677200248147
112Diallate13.73520043147
113Hexachlorobenzene13.788200284147
114Dimethoate13.85720087147
115Atrazine14.064200200147
1164-Aminobiphenyl14.17200169147
117Pentachlorophenol14.17200266147
118Pentachloronitrobenzene (Quintozene)14.213200237147
119Propyzamide14.377200173147
120Phenanthrene-d1014.477200188147
121n-Octadecane (C18)14.5220057147
122Phenanthrene14.52200178147
123Dinoseb14.616200211147
124Disulfoton14.61620088147
125Anthracene14.616200179147
126Carbazole14.961200167308
127Methyl parathion15.296200109308
128Di-n-butyl phthalate15.779200149308
1294-Nitroquinoline-N-oxide16.026200190308
130Parathion (ethyl parathion)16.075200291308
131Methapyrilene hydrochloride16.27320058308
132Isodrin16.52200193308
133Fluoranthene16.806200202308
134Benzidine17.124200184308
135Pyrene17.223200203308
136p-Terphenyl-d1417.627200244279
137Aramite isomer 217.627200175279
138Aramite isomer 117.818200135279
139p-Dimethylaminoazobenzene17.905200120279
140Chlorobenzilate18.041200251279
141Famphur18.487200218279
1423,3′-Dimethylbenzidine (o-tolidine)18.553200254159
143Kepone18.553200272279
144Benzyl butyl phthalate18.64200149279
145Bis(2-ethylhexyl)adipate18.89200129279
1462-Acetylaminofluorene19.015200181279
1474,4′-Methylene-bis(2-chloroaniline)19.561200231159
1483,3′-Dichlorobenzidine19.561200212279
149Benz[a]anthracene19.5612002281510
150Chrysene-d1219.5612002401510
151Chrysene19.612002261510
152Bis(2-ethylhexyl)phthalate19.8242001671510
1536-Methylchrysene20.4732002421510
154Di-n-octyl phthalate21.0312001491510
155Benzo[b]fluoranthene21.589200571510
1567,12-Dimethylbenz[a]anthracene21.5892002561510
157Benzo[k]fluoranthene21.6372002521510
158Benzo[a]pyrene22.2492002531510
159Perylene-d1222.3772002641510
1603-Methylcholanthrene23.082002681510
161Dibenz(a,h)acridine24.3572002791510
162Dibenz[a,j]acridine24.482002801510
163Indeno[1,2,3-cd]pyrene24.8822002771510
164Dibenz[a,h]anthracene24.9682002781510
165Benzo[g,h,i]perylene25.5372002761510

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

  1. 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.
  2. RMX GCカラムカタログ, GNBR4923A-JA, Restek Corporation, 2026.
GCカラム, 不活性, 低吸着
カラム内の活性点を抑えた、高感度・長寿命なカラム
お問い合わせ|Restek

関連製品


RMX-5Sil MS GCキャピラリーカラム, 30 m, 0.25 mm ID, 0.25 µm
Topaz, Single Taper Inlet Liner, 4.0 mm x 6.5 x 78.5, for Agilent GCs, w/Quartz Wool, Premium Deactivation, 5-pk.
Restek リークディテクタ
SVOC MegaMix 150 Kit, 1 mL/ampul; 6 ampuls/kit
GC-MS Tuning Mix, 1000 µg/mL, Methylene Chloride, 1 mL/ampul
Acid Surrogate Mix (4/89 SOW), 2000 µg/mL, Methanol, 1 mL/ampul
Base Neutral Surrogate Mix (4/89 SOW), 1000 µg/mL, Methylene Chloride, 1 mL/ampul
Revised SV Internal Standard Mix, 4000 µg/mL, Methylene Chloride, 1 mL/ampul

Authors

  • Jessi Collier

    Jessi is an advanced scientist in the GC applications group where her work focuses on environmental and food contaminants. Prior to joining Restek in 2023, she worked for the Mississippi State Chemical Lab as a pesticide residue analyst, primarily testing regulatory samples, agricultural samples, environmental samples, foods, and other consumer products via GC-MS, GC-MS/MS, GC-FID, and GC-ECD. Jessi holds a BS in chemistry and a BA in Mandarin Chinese from Mississippi State University.

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  • 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.

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  • Ramkumar Dhandapani

    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.

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  • 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.

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