气相色谱-串联质谱法测定得克隆及其相关化合物在土壤样品中的含量

引用本文: 刘合欢, 李会茹, 张文兵, 盛国英, 傅家谟, 彭平安. 气相色谱-串联质谱法测定得克隆及其相关化合物在土壤样品中的含量[J]. 分析化学, 2017, 45(3): 423-428. doi: 10.11895/j.issn.0253-3820.160656 shu

Citation: LIU He-Huan, LI Hui-Ru, ZHANG Wen-Bing, SHENG Guo-Ying, FU Jia-Mo, PENG Ping-An. Co-analysis of Dechlorane Plus and Related Compounds in Soil Sample by Gas Chromatography Coupled with Triple Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2017, 45(3): 423-428. doi: 10.11895/j.issn.0253-3820.160656 shu

气相色谱-串联质谱法测定得克隆及其相关化合物在土壤样品中的含量

1.
中国科学院广州地球化学研究所有机地球化学国家重点实验室, 广东省环境资源利用与保护重点实验室, 广州 510640;
2.
中国科学院大学, 北京 100049
基金项目:
本文系国家自然科学基金(No.41273002)、有机地球化学国家重点实验室专项基金(No.SKLOG2015A02)和广东省科技计划项目(No.2014B030301060)资助

摘要: 建立了得克隆(DP)及其脱氯产物和结构类似物等共11种化合物的气相色谱-串联质谱联用分析方法，并用于环境土壤中目标物的分析和污染特征研究。土壤样品抽提液经多段硅胶-氧化铝柱净化后，采用如下仪器条件分析：电子轰击电离源；选择反应离子对监测模式；DB-5HT毛细管柱(15 m×0.25 mm i. d.，0.1 μm)；进样口温度260℃，传输线温度280℃，离子源温度250℃；无分流进样1 μL，载气为氦气(1.5 mL/min)。实验结果表明，测定DP及其相关化合物的标准曲线线性范围为4~5个数量级，线性相关系数在0.9977~0.9999之间，仪器检出限在0.005~0.100 pg之间，方法检出限为0.25~5.00 fg/g，50 pg/μL标准样品平行5次进样的相对标准偏差(RSD)为1.1%~19.8%。对某典型污染区及其周边地区土壤进行分析，其中DP及相关化合物的总浓度在0.275~681 ng/g dw之间，检出率100%；单个目标物浓度在n.d.~537 ng/g dw之间，其中anti-DP和syn-DP为优势污染物，样品及质控样品中两种回收率指示物的加标回收率分别为55.0%~103.0%和83.4%~107.0%，空白/基质加标样品中目标物的平均回收率和RSD分别为53.9%~117.0%和6.0%~19.1%。

关键词:

English

Co-analysis of Dechlorane Plus and Related Compounds in Soil Sample by Gas Chromatography Coupled with Triple Tandem Mass Spectrometry

1.
State Key Laboratory of Organic Geochemistry and Guangdong Key Laboratory of Environmental Protection and Resources Utilization, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640, China;
2.
University of Chinese Academy of Science, Beijing 100049, China
Received Date: 05 September 2016
Revised Date: 13 January 2017
Fund Project:
This work was supported by the National Natural Science Foundation of China (No. 41273002), the Earmarked Fund of the State Key Laboratory of Organic Geochemicstry (No. SKLOD2015A02), and the Science and Technology Project of Guangdong Province, China (No. 2014B030301060)

Abstract: A co-analysis method of gas chromatography coupled to a triple quadrupole mass spectrometry (GC-MS/MS) was developed for the determination of 11 kinds of Dechlorane plus (DP) related compounds, including DPs, dechlorinated DPs and its structural analogs. This method was successfully applied to the analysis of DPs in field soil samples. After clean-up through a multi-layer silica/aluminum column, the soil sample concentrate was measured with the following instrumental parameters:electron impact ion source, select reaction monitoring mode, DB-5HT capillary column (15 m×0.25 mm i. d., 0.1 μm), and temperatures for injection port, transfer line and ion source were 260℃, 280℃ and 250℃, respectively. About 1 μL of sample was injected in splitless mode with helium at 1.5 mL/min as carrier gas. The results showed that the analyte standard curves demonstrated linearity of 4 or 5 magnitude ranges with the correlation coefficient varying between 0.9977 and 0.9999. The instrumental detection limits for these analytes were in the range of 0.005-0.100 pg, and the relative standard deviations (RSDs) for 5 parallel analyses at concentration level of 50 pg/μL were 1.1%-19.8%. With this method, the total concentrations of DP and related compounds in the field soil samples from a typical polluted site and its surrounding area changed between 0.275 and 681 ng/g dw (dry weight) with a detection rate of 100%, and the concentrations for individual analyte varied from n.d. to 537 ng/g dw with anti-DP and syn-DP as the dominant pollutants. The mean recoveries of the two surrogate standards in all samples were 55.0%-103.0% and 83.4%-107.0%, respectively, and the mean recoveries and RSDs of all analytes in blank and matrix samples were 53.9%-117.0% and 6.0%-19.1%, respectively.

Key words:

Dechlorane plus
/ Gass chromatography-tnadem mass spectrometry
/ Soil
/ Halogenated flame retardant
/ Pesistent organic pollutants

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气相色谱-串联质谱法测定得克隆及其相关化合物在土壤样品中的含量

English

Co-analysis of Dechlorane Plus and Related Compounds in Soil Sample by Gas Chromatography Coupled with Triple Tandem Mass Spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

气相色谱-串联质谱法测定得克隆及其相关化合物在土壤样品中的含量

English

Co-analysis of Dechlorane Plus and Related Compounds in Soil Sample by Gas Chromatography Coupled with Triple Tandem Mass Spectrometry

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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