气相色谱串联质谱法测定饮用水中多种农药及其代谢产物残留
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摘要
目的建立液液萃取-气相色谱串联质谱(Liquid liquid extraction and gas chromatography-tandem mass spectrometry,LLE-GC-MS/MS)测定饮用水中28种农药残留和代谢产物的检测方法。方法水样用二氯甲烷:正己烷(1∶1,V/V)溶剂提取后,合并提取液用氮气浓缩至1 ml,采用气相色谱串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)的多反应监测模式(multi reaction monitoring,MRM)对多种农药及其代谢产物残留同时定性定量分析,采用DB-5MS色谱柱(30 m×0.25 mm,0.25μm)分离。结果 28种农药在0.1~4.0 mg/L线性范围内均呈较好的线性关系,r>0.998。该方法的检出限为0.018~0.066μg/L。在1.6μg/L和4.0μg/L两种浓度添加水平,其平均回收率为85.3%~101.8%,相对标准偏差(relative standard deviations,RSD)为3.8%~9.2%。结论该方法快速、简单、准确,适用于同时检测饮用水中多种农药残留和代谢产物残留。
Objective To establish a method for the determination of 28 pesticides and metabolites residues in drinking water by Liquid extraction and gas chromatography-tandem mass spectrometry( LLE-GC-MS/MS). Methods The water samples were extracted with dichloromethane-hexane( 1∶ 1,V/V) and the extract was evaporated by nitrogen into 1. 00 ml. The 28 pesticides and metabolites residues were qualitative and quantitative analysis by gas chromatography-tandem mass spectrometry in multi reaction monitoring mode( MRM) and separated by DB-5 MS( 30 m × 0. 25 mm,0. 25 μm) column. Results The regression coefficients( r) of 28 pesticides were higher than 0. 998 and the limits of quantification( LOD) was 0. 018 ~ 0. 066 μg/L. At the 1. 6μg/L,4. 0 μg/L spiked level,the mean recoveries ranged from 85. 3% to 101. 8%,and the relative standard deviations( RSDs) ranged from 3. 8% to 9. 2%. Conclusion This method is fast,simple,high accuracy and has been used for the determination of 28 pesticides and metabolites residues in water samples.
Objective To establish a method for the determination of 28 pesticides and metabolites residues in drinking water by Liquid extraction and gas chromatography-tandem mass spectrometry( LLE-GC-MS/MS). Methods The water samples were extracted with dichloromethane-hexane( 1∶ 1,V/V) and the extract was evaporated by nitrogen into 1. 00 ml. The 28 pesticides and metabolites residues were qualitative and quantitative analysis by gas chromatography-tandem mass spectrometry in multi reaction monitoring mode( MRM) and separated by DB-5 MS( 30 m × 0. 25 mm,0. 25 μm) column. Results The regression coefficients( r) of 28 pesticides were higher than 0. 998 and the limits of quantification( LOD) was 0. 018 ~ 0. 066 μg/L. At the 1. 6μg/L,4. 0 μg/L spiked level,the mean recoveries ranged from 85. 3% to 101. 8%,and the relative standard deviations( RSDs) ranged from 3. 8% to 9. 2%. Conclusion This method is fast,simple,high accuracy and has been used for the determination of 28 pesticides and metabolites residues in water samples.
引文
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[9]李继革,王玉飞,施家威,等.固相萃取-气相色谱-串联质谱法测定水果中11种三唑类杀菌剂[J].色谱,2012,30(3):261-266.
[10]俞婧,周法东,李强,等.微波辅助提取-固相萃取净化-气相色谱-三重四级杆串联质谱法检测蔬菜中15种农药残留类持久性有机污染物[J].食品工业科技,2011,32(7):413-416.
[11]张敬平,刘文卫,周闰,等.气相色谱法同时检测生活饮用水中的27种有机磷农药残留[J].中国卫生检验杂志,2010,20(3):527-528.
[12]黄伟华,胡美华.全自动固相萃取-气质联用法测定水中14种农药残留[J].现代预防医学,2015,42(21):3965-3968.
[2]于桂兰,李万红.液液萃取-气相色谱质谱法测定饮用水中19种有机磷农药[J].中国卫生检验杂志,2012,22(6):1283-1285.
[3]李宏亮,詹铭,蒋志华,等.固相萃取-气相色谱法测定饮用水中12种农药[J].理化检验(化学分册),2014,52(12):1513-1516.
[4]高玲,杨元,景露,等.水中13种有机磷农药的固相萃取-气相色谱-质谱测定法[J].环境与健康杂志,2009,26(8):723-725.
[5]袁烁,曹之富,韦美蔓,等.气相色谱法测定水和土壤中8种菊酯类农药残留[J].北京农学院学报,2015,30(4):63-68.
[6]李晓晶,贺小平,黄聪,等.固相微萃取-气相色谱法同时测定饮用水中27种有机磷农药[J].中国卫生检验杂志,2009,19(6):1231-1233.
[7]袁鹏辉,陈明晓,董军,等.固相萃取-气相色谱/质谱选择离子检测法测定水中27种有机农药[J].分析试验室,2017,36(3):322-328.
[8]王雪平,闫凯.固相萃取-气相色谱-质谱法测定饮用水中15种农药残留量[J].理化检验(化学分册),2017,55(4):437-441.
[9]李继革,王玉飞,施家威,等.固相萃取-气相色谱-串联质谱法测定水果中11种三唑类杀菌剂[J].色谱,2012,30(3):261-266.
[10]俞婧,周法东,李强,等.微波辅助提取-固相萃取净化-气相色谱-三重四级杆串联质谱法检测蔬菜中15种农药残留类持久性有机污染物[J].食品工业科技,2011,32(7):413-416.
[11]张敬平,刘文卫,周闰,等.气相色谱法同时检测生活饮用水中的27种有机磷农药残留[J].中国卫生检验杂志,2010,20(3):527-528.
[12]黄伟华,胡美华.全自动固相萃取-气质联用法测定水中14种农药残留[J].现代预防医学,2015,42(21):3965-3968.