UPLC-串联质谱法快速测定地表水中多种农药残留
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摘要
采用超高效液相色谱-串联质谱法测定地表水中21种氨基甲酸酯和有机磷农药,通过优化试验条件,使方法在0. 500μg/L～100μg/L范围内线性良好,方法检出限为0. 1μg/L～6. 2μg/L。对空白水样做3个质量浓度水平的加标回收试验,5次测定结果的RSD为0. 3%～9. 5%,回收率为82. 0%～113%。将该方法用于测定徐州某地表水样品,3个水样均为未检出。
A method for determination of 21 pesticides in surface water by UPLC-MS-MS was developed. By optimizing the experimental conditions,good linearity was observed in the range of 0. 500 μg/L ～ 100 μg/L and the method detection limit was 0. 1 μg/L ～ 6. 2 μg/L. The RSDs of spiked samples with 5 repeated measurements in three concentration levels were 0. 3% ～ 9. 5% and the spiked recoveries were 82. 0% ～ 113%. The method was applied to detecting three surface water samples in Xuzhou,and the residues of all these pesticides were undetected.
A method for determination of 21 pesticides in surface water by UPLC-MS-MS was developed. By optimizing the experimental conditions,good linearity was observed in the range of 0. 500 μg/L ～ 100 μg/L and the method detection limit was 0. 1 μg/L ～ 6. 2 μg/L. The RSDs of spiked samples with 5 repeated measurements in three concentration levels were 0. 3% ～ 9. 5% and the spiked recoveries were 82. 0% ～ 113%. The method was applied to detecting three surface water samples in Xuzhou,and the residues of all these pesticides were undetected.
引文
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[10]杨晓松,余辉菊,马子元.固相膜萃取-高效液相色谱法测定饮用水中12种氨基甲酸酯类农药残留[J].中国卫生检验杂志,2012,22(7):1539-1541.
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[12]茅海琼,杜宇峰,叶文波,等.超高效液相色谱串联质谱法快速测定地表水和饮用水中6种氨基甲酸酯类农药[J].中国环境监测,2011,27(4):54-56.
[13] MAYERHELM B. Method development for the determination of52 pesticides in tobacco by liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography A,2009,1216(51):8953-8959.
[14]钱宗耀,刘河疆,张维维,等.固相微萃取-气相色谱法测定水中甲拌磷及其代谢产物残留[J].环境监测管理与技术,2017,29(1):50-52.
[15] RASTRELLI L,TOTARO K,SIMONE F D. Determination of organophosphorus pesticide residues in Cilento(Campania,Italy)virgin olive oil by cail Iary gas chromatography[J]. Food Chemistry,2002,79(3):303-305.
[2]朱月芳,尹艳敏,秦红兵.直接进样-超高效液相色谱串联质谱法同时测定水源水中9种农药[J].化学分析计量,2016,25(1):19-21.
[3]江阳,王艳,魏红,等.高效液相色谱-串联质谱法同时测定饮用水中的13种农药残留[J].中国卫生检验杂志,2016,26(2):184-188.
[4]环境保护部. HJ 168—2010环境监测分析方法标准制修订技术导则[S].北京:中国环境科学出版社,2010.
[5]环境保护部. HJ 827—2017水质氨基甲酸酯类农药的测定超高效液相色谱-三重四极杆质谱法[S].北京:中国环境科学出版社,2017.
[6]国家质量监督检验检疫总局. GB 14552—2003水、土壤中有机磷农药测定的气相色谱法[S].北京:中国质检出版社,2004.
[7]胡贝贞,郭伟强,陈笑梅.小麦中氨基甲酸酯类农药残留的HPLC-MS/MS测定方法研究[J].浙江大学学报(理学版),2007,34(4):426-431.
[8]王静,刘铮铮,钟光剑.超高效液相色谱-串联质谱法分析土壤及沉积物中氨基甲酸酯农药[J].中国环境监测,2013,29(4):103-106.
[9]陈贝,张胜军,冯元群,等.地表水中SVOCs和氨基甲酸酯类农药同步萃取技术的探讨[J].环境监测管理与技术,2016,28(6):51-54.
[10]杨晓松,余辉菊,马子元.固相膜萃取-高效液相色谱法测定饮用水中12种氨基甲酸酯类农药残留[J].中国卫生检验杂志,2012,22(7):1539-1541.
[11]李娟,赵永刚,丁曦宁.固相萃取/高效液相色谱法测定地表水中氨基甲酸酯类农药[J].环境监测管理与技术,2006,18(1):27-28.
[12]茅海琼,杜宇峰,叶文波,等.超高效液相色谱串联质谱法快速测定地表水和饮用水中6种氨基甲酸酯类农药[J].中国环境监测,2011,27(4):54-56.
[13] MAYERHELM B. Method development for the determination of52 pesticides in tobacco by liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography A,2009,1216(51):8953-8959.
[14]钱宗耀,刘河疆,张维维,等.固相微萃取-气相色谱法测定水中甲拌磷及其代谢产物残留[J].环境监测管理与技术,2017,29(1):50-52.
[15] RASTRELLI L,TOTARO K,SIMONE F D. Determination of organophosphorus pesticide residues in Cilento(Campania,Italy)virgin olive oil by cail Iary gas chromatography[J]. Food Chemistry,2002,79(3):303-305.