手性气相色谱质谱法测定莲藕及底泥中的多氯联苯对映体

引用本文: 戴守辉, 赵桦林, 王敏, Charles S. Wang, 柴婷婷, 杨曙明, 邱静. 手性气相色谱质谱法测定莲藕及底泥中的多氯联苯对映体[J]. 分析化学, 2012, 40(11): 1758-1763. doi: 10.3724/SP.J.1096.2012.20523 shu

Citation: DAI Shou-Hui, ZHAO Hua-Lin, WANG Min, Charles S. Wang, CHAI Ting-Ting, YANG Shu-Ming, QIU Jing. Determination of Polychlorinated Biphenyls Enantiomers in Lotus Root and Sediment by Chiral Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2012, 40(11): 1758-1763. doi: 10.3724/SP.J.1096.2012.20523 shu

手性气相色谱质谱法测定莲藕及底泥中的多氯联苯对映体

通讯作者: 邱静

基金项目:
本文系国家自然科学基金(No. 20907073)资助项目 (No. 20907073)

摘要: 采用气相色谱质谱(GC-MS)建立了莲藕、荷叶、荷茎及池塘底泥中6种手性多氯联苯(PCBs)PCB 91, 95, 136, 149, 176和183的分离分析方法。优化了对映体的仪器分离检测条件,考察了前处理中加速溶剂萃取(ASE)参数、提取剂以及净化方式等对方法的影响,最终确定采用正己烷-丙酮(1:1,V/V)在萃取温度100℃、压力10.3 MPa下静态提取10 min,提取液经H₂SO₄磺化后过Florisil小柱净化,洗脱液经浓缩并用异辛烷定容后,用分别配有Chirasil-Dex和BGB-172手性毛细管色谱柱的GC-MS检测。6种手性PCBs对映体的线性范围为0.5-100 μg/L,在0.25, 2.5和25 μg/kg添加浓度的回收率为82.8%-117.0%,相对标准偏差(RSD)为1.5%-13.6%,检出限为0.01-0.02 μg/kg,定量限为0.025-0.04 μg/kg。将本方法应用于实际样品的测定,在市售莲藕未检出6种手性PCBs,而污染区的莲藕、荷茎、荷叶及其生长底泥中均含有较高浓度手性PCBs,并且莲藕、荷茎和荷叶中PCB 91-2, PCB 95-1和(+)-PCB 136的浓度均高于其对映体,而PCB 149, 176和183的两个对映体之间均无显著的浓度差异。

关键词:

English

Determination of Polychlorinated Biphenyls Enantiomers in Lotus Root and Sediment by Chiral Gas Chromatography-Mass Spectrometry

1.
¹ Institute of Quality Standard & Testing Technology for Agro-Products, Key Laboratory of Agro-product Quality and Safety, Chinese Academy of Agricultural Sciences, Beijing 100081, China;

Corresponding author: 邱静

Received Date: 20 May 2012
Fund Project:
本文系国家自然科学基金(No. 20907073)资助项目

Abstract: An enantioselective method was developed for separation and determination of six chiral polychlorinated biphenyls (PCBs) including PCB 91, 95, 136, 149, 176 and 183 in lotus root, stem, leaf and sediment by GC-MS. After optimizations of instrumental parameters for enantiomeric separation and investigations of sample preparations including accelerated solvent extraction (ASE) parameters, extraction solvents and cleanup methods, PCBs enantiomers were extracted from samples by ASE with n-hexane/acetone (1:1, V/V) at 100℃ and 10.3 MPa for 10 min. The extracts were orderly sulphonated by sulfuric acid, purified by Florisil solid phase extraction column, reconstituted with isooctane after being concentrated, and respectively detected by GC-MS with Chirasil-Dex and BGB-172 columns. For all PCBs enantiomers, good linearities were obtained in the concentration range of 0.5-100 μg/L, and recoveries of spiked samples at 0.25, 2.5 and 25 μg/kg levels were 82.8%-117.0% with relative standard deviations (RSD) of 1.5%-13.6%. Limits of detection (LOD) and limits of quantification (LOQ) were 0.01-0.02 μg/kg and 0.025-0.04 μg/kg, respectively. The real samples analysis showed that chiral PCBs were not detected in lotus roots from markets, but higher concentrations were found in lotus root and sediment from contaminated area. The concentrations of PCB 91-2, PCB 95-1 and (+)- PCB 136 in lotus root, stem and leaf were respectively higher than those of their enantiomers, while no significant differences between two enantiomers of PCB 149, 176 and 183.

Key words:

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

手性气相色谱质谱法测定莲藕及底泥中的多氯联苯对映体

通讯作者: 邱静

English

Determination of Polychlorinated Biphenyls Enantiomers in Lotus Root and Sediment by Chiral Gas Chromatography-Mass Spectrometry

Corresponding author: 邱静

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

手性气相色谱质谱法测定莲藕及底泥中的多氯联苯对映体

通讯作者: 邱静

English

Determination of Polychlorinated Biphenyls Enantiomers in Lotus Root and Sediment by Chiral Gas Chromatography-Mass Spectrometry

Corresponding author: 邱静

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

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

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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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs