三重四级杆气相色谱串联质谱法测定水中20种指示性多氯联苯  

Analysis of 20 kinds of indicative polychlorinated biphenyls in water by gas chromatography-triple quadrupole mass spectrometry

作　　者：林华影[1] 阮国洪[2] 李一丹[1] 张伟[1] 林瑶[1] 张琼[1] UN Hua-ying;RUAN Guo-hong;LI Yi-dan;ZHANG Wei;LIN Yao;ZHANG Qiong(Fuzhou Center for Disease Control and Prevention, Fuzhou, Fujian 350004,China)

机构地区：[1]福州市疾病预防控制中心,福建福州350004 [2]福建医科大学公共卫生学院,福建福州350108

出　　处：《中国卫生检验杂志》2019年第10期1167-1171,共5页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立一种三重四级杆气相色谱串联质谱测定水中20种指示性多氯联苯的分析方法,优化色谱、质谱仪器及样品前处理条件。采用二级质谱检测技术,保证定性定量结果的可靠性,同时有效消除基体干扰。方法水样经ENVI-18固相萃取小柱提取,以乙酸乙酯、二氯甲烷洗脱,氮吹浓缩定容,用DB-5MS毛细管柱色谱分离,以三重四级杆气相色谱串联质谱多反应监测模式(MRM)进行测定,用内标法定量。结果能有效地分离检测水中20种指示性多氯联苯,方法的相对标准偏差<3.51%,各组分标准曲线的相关系数>0.9983,检出限为1.68ng/L^6.31ng/L,3个浓度水平的加标回收率为87.2%~105.1%。结论方法具有良好的选择性、灵敏度和准确度,化学背景低,对各种水样适应性好,用于水中20种指示性多氯联苯同时检测分析,结果令人满意。Objective A new method was developed and validated for the simultaneous analysis of 20 kinds of indicative polychlorinated biphenyls in water by gas chromatography coupled with triple quadrupole mass spectrometry, and the conditions of chromatographic, mass spectrometer, sample pretreatment were optimized. The second order mass spectra was adapted to increase the reliability of the results and eliminate the interference of the matrix. Methods The water sample was extracted on ENVI - 18 solid phase column and eluted with ethyl acetate, dichloromethane, then separated by GC with a DB - 5 MS capillary column. The exects was analyzed by gas chromatography coupled with triple quadrupole mass spectrometry ( GC - QqQ - MS /MS) using internal standard method. Results It is enable to easily and effectively separate and determinate 20 kinds of indicative polychlorinated biphenyls in water. In this method, broad linearity range, good linearity which correlation coefficient was greater than 0. 998 3, RF RSD was less than 3. 51%, the limits of quantification were within 1. 68 ng /L - 6. 31 ng /L, the recoveries determined at three concentration levels were within 87. 2%- 105. 1%. Conclusion This method is selective, sensitive and exact. It has low chemical background and good adaptility to various water samples. The results of this method are satisfactory for simultaneous determination of 20 kinds of indicative polychlorinated biphenyls in water.

关 键 词：水 指示性多氯联苯 气相色谱串联质谱法 

分 类 号：R123.1[医药卫生—环境卫生学]