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优化 GC-MS 分析多环芳烃 (PAH)

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  • 对于临界环境 PAH 化合物，Rxi-SVOCms 色谱柱可提供较好的分离效果和响应。
  • 柱流失低，可确保晚洗脱目标分析物的分析准确度。
  • 分流进样 SIM 分析可最大限度地减少进样歧视。
 

多环芳烃 (PAH) 是普遍存在的环境污染物，主要通过自然以及人类活动中含碳材料的不完全燃烧而形成。由于某些多环芳烃具有致癌性，因此空气、水和土壤样品的痕量监测对于暴露评估至关重要。在如下所示的优化条件下，利用 Rxi-SVOCms 色谱柱通过 GC-MS 分析 PAH，可有效检测最相关的化合物。

采用 SIM 模式和分流进样，可最大限度减少具有挑战性的煤焦油样品的进样歧视，从而在分析多种 PAH 化合物时观察到良好的色谱性能。分析挥发性早洗脱化合物时可获得良好的峰形和响应，而低柱流失可最大限度减少背景干扰并提高晚洗脱化合物的分析灵敏度。此外，Rxi-SVOCms 色谱柱的柱效和选择性可确保良好分离苯并[b]荧蒽和苯并[k]荧蒽等同重 PAH。同时，也可较好地分离茚并[123-cd]芘和二苯并[ah]蒽（即使响应不成比例），这减少了出现偏差结果和假阳性报告的可能性。 

图 1: Rxi-SVOCms 色谱柱的柱效和选择性可确保通过 GC-MS 分析 PAH时，出色分离 临界物质对。

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GC_EV1606
PeakstR (min)
1.Naphthalene6.27
2.2-Methylnaphthalene7.09
3.1-Methylnaphthalene7.21
4.Biphenyl7.66
5.2,6-Dimethylnaphthalene7.84
6.Acenaphthylene8.17
7.(IS) Acenaphthene-d108.35
8.Acenaphthene8.39
9.2,3,5-Trimethylnaphthalene8.86
10.Fluorene9.02
11.Dibenzothiophene10.03
12.(IS) Phenanthrene-D1010.16
13.Phenanthrene10.19
PeakstR (min)
14.Anthracene10.25
15.1-Methylphenanthrene10.95
16.Fluoranthene11.65
17.Pyrene11.92
18.Benz[a]anthracene13.46
19.(IS) Chrysene-D1213.47
20.Chrysene13.51
21.Benzo[b]fluoranthene*15.14
22.Benzo[k]fluoranthene15.19
23.(SS) Benzo[a]pyrene-d1215.66
24.Benzo[a]pyrene15.70
25.Indeno[1,2,3-cd]pyrene17.78
26.Dibenz[a,h]anthracene17.83
27.Benzo[ghi]perylene18.27
* Benzo[b]fluoranthene and benzo[j]fluoranthene coelution.
ColumnRxi-SVOCms, 30 m, 0.25 mm ID, 0.25 µm (cat.# 16623)
Standard/SampleNIST SRM 1597a - complex mixture of polycyclic aromatic hydrocarbons from coal tar
Diluent:Dichloromethane
Injection
Inj. Vol.:1 µL split (split ratio 20:1)
Liner:Topaz 4.0 mm ID single taper inlet liner with wool (cat.# 23303)
Inj. Temp.:250 °C
Split Vent Flow Rate:24 mL/min
Oven
Oven Temp.:40 °C (hold 0.5 min) to 280 °C at 20 °C/min to 330 °C at 6 °C/min (hold 4 min)
Carrier GasHe, constant flow
Flow Rate:1.2 mL/min
DetectorMS
Mode:SIM
SIM Program:
GroupStart Time
(min)		Ion(s) (m/z)Dwell (ms)
15.00127.05, 128.05, 129.00 10
26.75115.10, 139.00, 141.00, 142.05 10
37.47141.00, 152.00, 153.05, 154.05, 155.05, 156.10, 162.10, 164.10 10
48.03150.00, 151.05, 152.05, 153.05, 154.10, 162.10, 164.10 10
58.66153.05, 155.10, 163.05, 164.10, 165.05, 166.05, 169.10, 170.10 10
69.62139.00, 151.95, 176.10, 177.10, 178.10, 179.10, 183.95, 185.00, 188.10, 189.10 10
710.71189.05, 190.05, 191.10, 192.10 10
811.37200.10, 201.10, 202.10, 203.05 10
911.81200.10, 201.05, 202.05, 203.05 10
1012.84114.00, 120.00, 226.10, 227.10, 228.10, 229.10, 240.10 10
1114.44126.00, 132.00, 250.10, 252.10, 253.10, 264.00 10
1215.51126.00, 132.00, 250.05, 252.05, 253.05, 264.00 10
1316.95137.95, 139.00, 274.05, 276.10, 277.10, 278.10, 279.10 10
1418.10138.00, 274.05, 276.10, 277.10 10
Transfer Line Temp.:280 °C
Analyzer Type:Quadrupole
Source Type:Extractor
Extractor Lens:6 mm ID
Source Temp.:330 °C
Quad Temp.:150 °C
Tune Type:DFTPP
Ionization Mode:EI
InstrumentAgilent 7890B GC & 5977A MSD
Sample PreparationNIST SRM 1597a was diluted 5x in dichloromethane. Isotope-labeled IS/SS are 20 pg on-column. Samples were aliquoted into amber 2 mL, 9 mm short-cap, screw-thread vials (cat.# 21143) containing glass Big Mouth inserts (cat.# 21782) and sealed with 2.0 mL, 9 mm short-cap, screw-vial closures (cat.# 23842).
NotesThe internal standard and surrogate standard mass on column is 20 pg.
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EVFA3822A-CN