电子制冷预浓缩-双柱气相色谱-质谱/氢火焰检测器法测定空气中104种挥发性有机物

引用本文: 张烃, 张翼翔, 杜祯宇, 刀谞, 张秀蓝, 曹冠, 贾岳清, 杜世娟, 汤卡, 单丹滢, 周昊, 周瑞. 电子制冷预浓缩-双柱气相色谱-质谱/氢火焰检测器法测定空气中104种挥发性有机物[J]. 色谱, 2019, 37(4): 418-425. doi: 10.3724/SP.J.1123.2018.12022 shu

Citation: ZHANG Ting, ZHANG Yixiang, DU Zhenyu, DAO Xu, ZHANG Xiulan, CAO Guan, JIA Yueqing, DU Shijuan, TANG Ka, SHAN Danying, ZHOU Hao, ZHOU Rui. Determination of 104 volatile organic compounds in air by double column gas chromatography-mass spectrometry/flame ionization detector coupled with electronically controlled cryo-focusing unit[J]. Chinese Journal of Chromatography, 2019, 37(4): 418-425. doi: 10.3724/SP.J.1123.2018.12022 shu

电子制冷预浓缩-双柱气相色谱-质谱/氢火焰检测器法测定空气中104种挥发性有机物

张烃 ^1, ,
张翼翔 ^1, ,
杜祯宇 ^1, ,
刀谞 ^2, ,
张秀蓝 ^1, ,
曹冠 ^1, ,
贾岳清 ^1, ,
杜世娟 ^3, ,
汤卡 ^1, ,
单丹滢 ^1, ,
周昊 ^1, ,
周瑞 ^1,

1.
国家环境分析测试中心, 北京 100029;
2.
中国环境监测总站, 北京 100012;
3.
岛津企业管理(中国)有限公司北京分公司, 北京 100020
基金项目:
国家重点研发计划项目课题（2016YFC0206204）.

摘要: 基于吸附剂辅助电子制冷预浓缩技术，建立了多维切割双柱气相色谱-质谱/氢火焰离子化检测器（GC-MS/FID）同时测定环境空气中104种挥发性有机物（VOCs）的方法。将采集于苏玛罐中的环境空气样品在配有吸附剂的电子制冷预浓缩系统中富集、脱附、除水、除CO₂和浓缩，然后通过GC-MS/FID的多维切割单元将C₂~C₃组分和C₄~C₁₂组分分别引入PLOT柱和InterCap-624柱进行分离。C₂~C₃组分用FID检测，以保留时间定性、外标法定量；C₄~C₁₂组分采用电子轰击离子源质谱检测，以保留时间和特征离子定性、内标法定量。考察了冷阱吸附剂种类、辅助压力控制单元压力设置、双柱切换时间切割点等参数对分析结果的影响，优化了GC-MS/FID条件，并评估了在此优化条件下的方法性能。104种VOCs在0.0446~0.892 μmol/m³范围内线性关系良好，相关系数（r）为0.9984~0.9999，对0.0446 μmol/m³和0.223 μmol/m³水平的混合标准气体重复6次进样，平均回收率为86.4%~116.1%，相对标准偏差为0.9%~11.3%；方法的检出限为0.145~1.90 μg/m³，定量限为0.435~5.70 μg/m³。该法稳定性好，灵敏度高，操作简便，可用于环境空气中104种VOCs的测定。

关键词:

English

Determination of 104 volatile organic compounds in air by double column gas chromatography-mass spectrometry/flame ionization detector coupled with electronically controlled cryo-focusing unit

1.
National Research Center for Environmental Analysis and Measurements(CNEAC), Beijing 100029, China;
2.
China National Environmental Monitoring Center(CNEMC), Beijing 100012, China;
3.
Beijing Branch, Shimadzu(China) Co. Ltd, Beijing 100020, China
Received Date: 14 December 2018
Fund Project:
National Key Research and Development Plan (No. 2016YFC0206204).

Abstract: A method for the determination of 104 volatile organic compounds (VOCs) in ambient air based on double column multi dean switching gas chromatography-mass spectrometry/flame ionization detector (GC-MS/FID) coupled with sorbent assisted electronically controlled cryo-focusing unit was developed and evaluated. The sorbent assisted electronically controlled cryo-focusing unit was used for trapping, dehydration and focusing of VOCs sampled in summa canisters. The VOCs were split into two parts by the multi dean switching unit in GC-MS/FID. The C₂-C₃ components were determined in a PLOT capillary column with an FID detector, while the C₄-C₁₂ components were determined in an Intercap-624 capillary column with a MS detector. The C₂-C₃ components were qualitatively confirmed from the retention time and quantified by the calibration curves, while the C₄-C₁₂ components were qualitatively confirmed from the retention time and the relative abundance ratio of characteristic ions, and quantified by the internal standard calibration curves. The major factors influencing the cryo-focusing performance including the type of sorbent tube, the pressure employed in assisted pressure control unit (APC), and the split point in multi dean switching unit were investigated. The chromatographic and MS parameters were optimized. Under optimum conditions, a linear relationship was observed with the content of VOCs ranging from 0.0446 to 0.892 μmol/m³, and correlation coefficients (r) no less than 0.9984. The average spiked recoveries of the six VOCs at two levels of 0.0446 μmol/m³ and 0.223 μmol/m³ were 86.4%-116.1%, with relative standard deviations in the range of 0.9%-11.3% The method detection limits (MDLs) and the limits of quantification (LOQs) were 0.145-1.90 μg/m³ and 0.435-5.70 μg/m³, respectively. The method is accurate, sensitive and simple, and is suitable for the determination of the 104 VOCs in ambient air.

Key words:

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电子制冷预浓缩-双柱气相色谱-质谱/氢火焰检测器法测定空气中104种挥发性有机物

English

Determination of 104 volatile organic compounds in air by double column gas chromatography-mass spectrometry/flame ionization detector coupled with electronically controlled cryo-focusing unit

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

电子制冷预浓缩-双柱气相色谱-质谱/氢火焰检测器法测定空气中104种挥发性有机物

English

Determination of 104 volatile organic compounds in air by double column gas chromatography-mass spectrometry/flame ionization detector coupled with electronically controlled cryo-focusing unit

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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