超声提取/超高效液相色谱-串联质谱法测定土壤中乙酰甲胺磷与甲胺磷的研究
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摘要
建立了超声提取/超高效液相色谱-三重四极杆串联质谱(UPLC-MS/MS)快速测定土壤中乙酰甲胺磷和甲胺磷的方法。10. 0 g土壤样品采用20. 0 m L甲醇超声萃取30 min,取上清液过0. 22μm滤膜后进行UPLC-MS/MS分析,外标法定量。结果表明:乙酰甲胺磷和甲胺磷在0. 002～20. 0μg/L质量浓度范围内线性良好(r~2> 0. 999),方法检出限分别为0. 004 9μg/kg和0. 003 4μg/kg。在0. 400、4. 00、40. 00μg/kg加标水平下,土壤样品中乙酰甲胺磷和甲胺磷的平均回收率分别为83. 0%～91. 5%和88. 0%～94. 8%,相对标准偏差(RSD,n=6)分别为2. 3%～4. 8%和1. 8%～4. 2%。该方法前处理简单快捷、灵敏度高、定性定量准确,可用于土壤样品中乙酰甲胺磷和甲胺磷含量的快速检测。
A method was developed for the determination of acephate and methamidophos in soil by ultrahigh performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS) with ultrasonic extraction. 10. 0 g soil sample was extracted with 20. 0 m L methanol under ultrasonic assistance for 30 min. Then the clear supernatant extract was filtered through 0. 22 μm membrane,and analyzed by UPLC-MS/MS with external standard method. There were good linear relationships for acephate and methamidophos both in the range of 0. 002-20. 0 μg/L with their correlation coefficients( r~2) larger than 0. 999. The detection limits for acephate and methamidophos in soil were0. 004 9 μg/kg and 0. 003 4 μg/kg,respectively. The recoveries for acephate and methamidophos at three spiked levels of 0. 400,4. 00 and 40. 00 μg/kg were in the ranges of 83. 0%-91. 5% and88. 0%-94. 8% with their relative standard deviations( RSDs,n = 6) of 2. 3%-4. 8% and 1. 8%-4. 2%,respectively. The method was simple,rapid,sensitive and accurate in both quantitation and qualitation,and was suitable for the routine determination of acephate and methamidophos in soil samples.
A method was developed for the determination of acephate and methamidophos in soil by ultrahigh performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS) with ultrasonic extraction. 10. 0 g soil sample was extracted with 20. 0 m L methanol under ultrasonic assistance for 30 min. Then the clear supernatant extract was filtered through 0. 22 μm membrane,and analyzed by UPLC-MS/MS with external standard method. There were good linear relationships for acephate and methamidophos both in the range of 0. 002-20. 0 μg/L with their correlation coefficients( r~2) larger than 0. 999. The detection limits for acephate and methamidophos in soil were0. 004 9 μg/kg and 0. 003 4 μg/kg,respectively. The recoveries for acephate and methamidophos at three spiked levels of 0. 400,4. 00 and 40. 00 μg/kg were in the ranges of 83. 0%-91. 5% and88. 0%-94. 8% with their relative standard deviations( RSDs,n = 6) of 2. 3%-4. 8% and 1. 8%-4. 2%,respectively. The method was simple,rapid,sensitive and accurate in both quantitation and qualitation,and was suitable for the routine determination of acephate and methamidophos in soil samples.
引文
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[6] Wu X. Chin. J. Health Lab. Technol.(吴璇.中国卫生检验杂志),2013,23(2):520-522.
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[8] He M,Tie B Q,Dai R C,Chen L,Yu P Z. Agrochemicals(贺敏,铁柏清,戴荣彩,陈莉,余平中.农药),2008,47(2):122-124.
[9] Ma H Z,Pan L G,Li A,Zhang Z Y. J. Food Saf. Qual.(马红枣,潘立刚,李安,张志勇.食品安全质量检测学报),2017,8(2):481-485.
[10] Wang L. Ningxia J. Agric. Fores. Sci. Technol.(王玲.宁夏农林科技),2011,52(12):231-232.
[11] Yu L. Agrochemicals(于力.农药),1996,35(10):11-12.
[12] Zhang Y,Luo Q. Agric. Dev. Equip.(张莹,罗茜.农业开发与装备),2013,(3):56.
[13] Yang K L,Xie C L. Appl. Chem. Ind.(杨开莲,谢承礼.应用化工),2007,36(4):407-408.
[14] Zhang M S,Li T Y,He S H,Liang Y. J. Instrum. Anal.(张鸣珊,李腾崖,何书海,梁焱.分析测试学报),2016,35(9):1195-1198.
[15] HJ 168-2010. Environmental Monitoring-Technical Guideline on Drawing and Revising Analytical Method Standards.Environmental Protection Professional Standard of the People's Republic of China(环境监测分析方法标准制修订技术导则.中华人民共和国环境保护行业标准).