气相色谱-电子捕获负化学电离-质谱法测定电子电气产品聚合物材料中的中链氯化石蜡
Determination of Medium Chain Chlorinated Paraffins in Polymer Materials for Electrical and Electronic Products by GC-ECNCI-MS
摘 要
1.000 0 g样品用10 mL正己烷超声萃取90 min，提取液用于气相色谱-电子捕获负化学电离-质谱法分析。仪器工作条件如下：进样口温度为280℃，离子源温度为180℃，甲烷气流量为2.0 mL·min-1。采用多元线性回归法，建立了m/z 370和m/z 384离子峰面积与中链氯化石蜡（MCCPs）总量的线性回归方程，该方程可对质量浓度范围为10.0~100 mg·L-1的MCCPs进行较准确的定量。采用此方法分析了10批次电子电气产品聚合物材料样品，其中2批次样品中检出MCCPs，其质量比分别为2 081，4 165 mg·kg-1。
中链氯化石蜡
电子电气产品
多元线性回归
GC-ECNI-MS
medium chain chlorinated paraffin
electrical and electronic product
multiple linear regression calibration
Abstract
The sample (1.000 0 g) was extracted ultrasonically with 10 mL of haxane for 90 min. The extract was separated and analyzed by gas chromatography-electron capture negative chemical ionization-mass spectrometry (GC-ECNI-MS). The optimum conditions were as follow:280℃ of inlet temperature, 180℃ of ion source temperature and 2.0 mL·min-1 of methane flow rate. Linear regression equation between the total medium chain chlorinated paraffins (MCCPs) and peak areas of ions m/z 370, m/z 384 was established by applying the multiple linear regression calibration. The equation allowed accurate quantification of MCCPs in the range of 10.0-100 mg·L-1. The proposed method was used to determine MCCPs in 10 batches of polymer materials for electrical and electronic products, and MCCPs were found in 2 batches of samples, with mass ratio of 2 081, 4 165 mg·kg-1, respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201712001
所属栏目 试验与研究
基金项目 广东省质量技术监督局科技项目（2014PJ03）
收稿日期 2016/11/10
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备注冯岸红(1987-),女,广东惠州人,硕士研究生,主要从事有害物质检测研究工作,fah814@163.com
引用该论文: FENG Anhong,XING Yuanna,YE Linquan,LIN Zhihui,CHEN Zeyong. Determination of Medium Chain Chlorinated Paraffins in Polymer Materials for Electrical and Electronic Products by GC-ECNCI-MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(12): 1365～1369
冯岸红,幸苑娜,叶淋泉,林志惠,陈泽勇. 气相色谱-电子捕获负化学电离-质谱法测定电子电气产品聚合物材料中的中链氯化石蜡[J]. 理化检验－化学分册, 2017, 53(12): 1365～1369
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参考文献
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【10】TOMY G T, STERN G A. Analysis of C14-C17 polychloro-n-alkanes in environmental matrixes by accelerated solvent extraction-high-resolution gas chromatography/electron capture negative ion high-resolution mass spectrometry[J]. Analytical Chemistry, 1999,71(21):4860-4865.
【11】RETH M, ZENCAK Z, OEHME M. New quantification procedure for the analysis of chlorinated paraffins using electron capture negative ionization mass spectrometry[J]. Journal of Chromatography A, 2005,1081(2):225-231.
【12】幸苑娜,冯岸红,叶淋泉,等.混合氯化石蜡中短链氯化石蜡定量分析方法的比较[J].色谱, 2016,34(3):346-350.
【2】CHEN M Y, LUO X J, ZHANG X L, et al. Chlorinated paraffins in sediments from the Pearl River Delta, South China:Spatial and temporal distributions and implication for processes[J]. Environmental Science & Technology, 2011,45(23):9936-9943.
【3】RENBERG L, SUNDSTRÖM G, SUNDH-NYGÅRD K. Partition coefficients of organic chemicals derived from reversed phase thin layer chromatography[J]. Chemosphere, 1980,9(11):683-691.
【4】BARBER J L, SWEETMAN A J, THOMAS G O, et al. Spatial and temporal variability in air concentra-tions of short-chain (C10-C13) and medium-chain (C14-C17) chlorinated n-alkanes measured in the UK atmosphere[J]. Environmental Science & Technology, 2005,39(12):4407-4415.
【5】HOUDE M, MUIR D C G, TOMY G T, et al. Bioaccumulation and trophic magnification of short-and medium-chain chlorinated paraffins in food webs from lake ontario and lake michigan[J]. Environmental Science & Technology, 2008,42(10):3893-3899.
【6】PRIBYLOVÁ P, KLÁNOVÁ J, HOLOUBEK I. Screening of short-and medium-chain chlorinated paraffins in selected riverine sediments and sludge from the Czech Republic[J]. Environmental Pollution, 2006,144(1):248-254.
【7】RETH M, ZENCAK Z, OEHME M. First study of congener group patterns and concentrations of short-and medium-chain chlorinated paraffins in fish from the North and Baltic Sea[J]. Chemosphere, 2005,58:847-854.
【8】THOMAS G O, FARRAR D, BRAEKEVELT E, et al. Short and medium chain length chlorinated paraffins in UK human milk fat[J]. Environment International, 2006,32(1):34-40.
【9】Risk assessment part Ⅱ-Human health of C14-C17 polychloro-n-alkanes[EB/OL].[2016-11-10]. http://publications.jrc.ec.europa.eu/repository/bitstream/JRC66049/lbna25202enn.pdf.
【10】TOMY G T, STERN G A. Analysis of C14-C17 polychloro-n-alkanes in environmental matrixes by accelerated solvent extraction-high-resolution gas chromatography/electron capture negative ion high-resolution mass spectrometry[J]. Analytical Chemistry, 1999,71(21):4860-4865.
【11】RETH M, ZENCAK Z, OEHME M. New quantification procedure for the analysis of chlorinated paraffins using electron capture negative ionization mass spectrometry[J]. Journal of Chromatography A, 2005,1081(2):225-231.
【12】幸苑娜,冯岸红,叶淋泉,等.混合氯化石蜡中短链氯化石蜡定量分析方法的比较[J].色谱, 2016,34(3):346-350.
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