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
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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>0.998 3,检出限为1.68 ng/L～6.31 ng/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.
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.
引文
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[13] 卞战强,查玉娥,于健,等.水中16种半挥发性农药的膜式固相萃取-气相色谱-质谱测定法[J].环境与健康杂志,2014,31(4):339-341.
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[2] 黎莉,黄晶,曹旭静,等.土壤中多氯联苯分析方法研究进展[J].污染防治技术.2011(2):16-20.
[3] 刘敏霞,杨玉义,李庆孝,等.中国近海海洋环境多氯联苯(PCBs)污染现状及影响因素[J].环境科学,2013,34(8):3309-3315.
[4] 吉仙枝,王华芳.食品中多氯联苯检测方法的评价[J].洛阳师范学院学报,2014(8):54-56.
[5] 管玉峰,岳强,涂秀云,等.珠江入海口水体中多氯联苯的分布特征及其来源分析[J].环境科学研究,2011,24(8):865-872.
[6] 蒋慧,赵力,娄彩荣,等.环境中多氯联苯(PCBs)的分析方法研究[J].四川环境,2010,29(6):147-150.
[7] 艾连峰,李玮,王敬,等.气相色谱-串联质谱法测定牛奶中多氯联苯及多环芳烃[J].分析测试学报,2015,34(5):570-575.
[8] 杨素娜,陆华.气相色谱法、气质联用法测定土壤中多氯联苯[J].环境科学导刊,2013,32(5):121-124.
[9] 曾少林,干宁,侯建国,等.环境样品中痕量多氯联苯的前处理方法及萃取材料的研究进展[J].岩矿测试,2012,31(3):399-406.
[10] 刘金巍,王磊,安彩秀,等.固相萃取-气相色谱法测定饮用水中的多氯联苯[J].岩矿测试,2011,30(5):611-616.
[11] 张丽,刘玉侠.固相萃取-高效液相色谱法同时测定饮用水中苯胺和联苯胺[J].环境监测管理与技术,2013,25(5):41-43.
[12] 朱铭洪.固相萃取-气质联用测定环境水样中5种痕量土霉味物质[J].中国卫生检验杂志,2014,24(10):1393-1395.
[13] 卞战强,查玉娥,于健,等.水中16种半挥发性农药的膜式固相萃取-气相色谱-质谱测定法[J].环境与健康杂志,2014,31(4):339-341.
[14] 史永富,蔡友琼,于慧娟,等.气相色谱串联质谱法用于水产品中多氯联苯二代污染物鉴别[J].分析化学,2014,42(11):1640-1645.
[15] 施家威,李继革,王玉飞,等.固相萃取-气相色谱/三重四极杆串联质谱分析蔬菜中43种农药残留[J].色谱,2010,28(12):1137-1143.