大体积采样结合高分辨气相色谱-电子捕获负化学源-低分辨质谱法测定空气中的短链氯化石蜡

doi:10.3724/SP.J.1123.2015.08032

色谱 ›› 2016, Vol. 34 ›› Issue (2): 202-208.DOI: 10.3724/SP.J.1123.2015.08032

大体积采样结合高分辨气相色谱-电子捕获负化学源-低分辨质谱法测定空气中的短链氯化石蜡

史蕾蒙^1,2, 高媛², 侯晓虹¹, 张海军², 张亦弛², 陈吉平^1,2

1. 沈阳药科大学, 辽宁沈阳 110016;
2. 中国科学院大连化学物理研究所, 辽宁大连 116023

收稿日期:2015-08-27 出版日期:2016-02-08 发布日期:2012-09-11
通讯作者: 陈吉平
基金资助:
国家自然科学基金项目(21307128,21337002).

Determination of short-chain chlorinated paraffins in ambient air using high-volume sampling combined with high resolution gas chromatography-electron capture negative ion-low resolution mass spectrometry

SHI Leimeng^1,2, GAO Yuan², HOU Xiaohong¹, ZHANG Haijun², Zhang Yichi², CHEN Jiping^1,2

1. Shenyang Pharmaceutical University, Shenyang 110016, China;
2. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China

Received:2015-08-27 Online:2016-02-08 Published:2012-09-11
Supported by:
National Natural Science Foundation of China (Grant Nos. 21307128, 21337002).

摘要/Abstract

摘要：

建立了大体积采样结合高分辨气相色谱-电子捕获负化学源-低分辨质谱(HRGC-ECNI-LRMS)测定空气中短链氯化石蜡(SCCPs)的定量分析方法。联合使用酸化硅胶复合层析柱和碱性氧化铝层析柱净化处理空气样品中的SCCPs,并对净化条件进行优化。使用该方法计算得到氯含量为58.1%~63.3%的SCCPs系列标准储备溶液的总响应因子与氯含量线性相关,相关系数(R²)大于0.99。该方法的仪器检出限(S/N≥3)为4.2 pg,定量限(S/N≥10)为12 pg。SCCPs的方法检出限(MDL)为0.34 ng/m³(n=7),实际样品加标回收率均达80%以上。该方法灵敏度高、选择性好,能满足空气样品中SCCPs的监测和分析需求。

关键词: 大体积采样, 短链氯化石蜡, 高分辨气相色谱-电子捕获负化学源-低分辨质谱, 空气

Abstract:

An analytical method for quantifying short-chain chlorinated paraffins (SCCPs) in ambient air using high-volume sampling combined with high resolution gas chromatography-electron capture negative ion-low resolution mass spectrometry (HRGC-ECNI-LRMS) was developed. An acidified silica gel column and a basic alumina column were used to optimize the cleanup procedures. The results showed a good linearity (R²＞0.99) between the total response factors and the degree of chlorination of SCCPs in the content range of 58.1%-63.3%. The limits of detection (S/N≥3) and the limits of quantification (S/N≥10) were 4.2 and 12 pg, respectively. The method detection limit (MDL) for SCCPs was 0.34ng/m³ (n=7). The recoveries of SCCPs in air samples were in the range of 81.9% to 94.2%. It is demonstrated that the method is suitable for the quantitative analysis of SCCPs in air samples.

Key words: air, high resolution gas chromatography-electron capture negative ion-low resolution mass spectrometry (HRGC-ECNI-LRMS), high-volume sampling, short-chain chlorinated paraffins (SCCPs)

中图分类号:

O658

史蕾蒙, 高媛, 侯晓虹, 张海军, 张亦弛, 陈吉平. 大体积采样结合高分辨气相色谱-电子捕获负化学源-低分辨质谱法测定空气中的短链氯化石蜡[J]. 色谱, 2016, 34(2): 202-208.

SHI Leimeng, GAO Yuan, HOU Xiaohong, ZHANG Haijun, Zhang Yichi, CHEN Jiping. Determination of short-chain chlorinated paraffins in ambient air using high-volume sampling combined with high resolution gas chromatography-electron capture negative ion-low resolution mass spectrometry[J]. Chinese Journal of Chromatography, 2016, 34(2): 202-208.

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大体积采样结合高分辨气相色谱-电子捕获负化学源-低分辨质谱法测定空气中的短链氯化石蜡

Determination of short-chain chlorinated paraffins in ambient air using high-volume sampling combined with high resolution gas chromatography-electron capture negative ion-low resolution mass spectrometry

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