液相色谱串联质谱法测定水果中多菌灵残留量
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摘要
为建立一种测定苹果、猕猴桃、脐橙等水果中多菌灵残留量的液相色谱串联质谱检测方法,在弱碱性条件下采用乙酸乙酯振荡提取, MCX固相萃取柱净化,用液相色谱串联质谱仪测定,外标法定量。结果表明,多菌灵在5.0～200 ng/mL范围内呈良好的线性关系,线性相关系数为0.999 9;在10.0, 20.0和40.0μg/kg浓度水平下,添加回收率范围为88.2%～100.5%,相对标准偏差RSD (n=6)为2.05%～8.78%,方法定量限为0.01 mg/kg。
A method was developed for the determination of carbendazim residues in fruits such as apple, kiwifruit and navel orange by liquid chromatography-tandem mass spectrometry(LC-MS/MS). Under weak alkaline conditions, the sample was extracted with ethyl acetate and purified by MCX column, determined by liquid chromatography-tandem mass spectrometry(LC-MS/MS) and quantified by external standard method. The results showed that carbendazim had a good linear relationship in the range of 5.0 ng/mL to 200 ng/mL, the linear correlation coefficient was 0.999 9, the recovery ranged from 88.2% to100.5% at the levels of 10.0, 20.0 and 40.0 μg/kg, and the relative standard deviation RSD of precision was 2.05% to 8.78%(n=6). The quantitative limit of the method was 0.01 mg/kg.
A method was developed for the determination of carbendazim residues in fruits such as apple, kiwifruit and navel orange by liquid chromatography-tandem mass spectrometry(LC-MS/MS). Under weak alkaline conditions, the sample was extracted with ethyl acetate and purified by MCX column, determined by liquid chromatography-tandem mass spectrometry(LC-MS/MS) and quantified by external standard method. The results showed that carbendazim had a good linear relationship in the range of 5.0 ng/mL to 200 ng/mL, the linear correlation coefficient was 0.999 9, the recovery ranged from 88.2% to100.5% at the levels of 10.0, 20.0 and 40.0 μg/kg, and the relative standard deviation RSD of precision was 2.05% to 8.78%(n=6). The quantitative limit of the method was 0.01 mg/kg.
引文
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[13]蔡世炎,游文玮,李耀群.导数同步荧光法快速检测香菇中的多菌灵[J].分析测试学报,2007,26(1):117-119.
[2]王奕.欧盟要逐步淘汰草铵膦、敌草快、多菌灵等,国内要接轨?[J].营销界(农资与市场),2016(2):67-68.
[3]中华人民共和国农业部.对十二届全国人大四次会议第7307号建议的答复(关于修订多菌灵相关标准)[Z].2016-08-26.
[4]中华人民共和国卫生部.蔬菜﹑水果中甲基托布津﹑多菌灵的测定:GB/T 5009.188-2003[S].北京:中国标准出版社,2003.
[5]中华人民共和国卫生部.水果蔬菜中多菌灵残留的测定高效液相色谱法:GB/T 23380-2009[S].北京:中国标准出版社,2009.
[6]中华人民共和国农业部.蔬菜水果中多菌灵等4种苯并咪唑类农药残留量的测定高效液相色谱法:NY/T 1680-2009[S].北京:中国标准出版社,2009.
[7]廖涛,杨玉平,程薇,等.苹果中多菌灵、噻菌灵和甲基托布津的高效液相色谱法分析[J].分析测试技术与仪器,2010,16(4):257-261.
[8]陈莹,丛佩华.水果中多菌灵农药残留检测方法的比较与基质效应研究[J].分析试验室,2008,27:408-412.
[9]游子涵,陈智东,柳训才,等.油菜植株及其土壤中多菌灵残留检测及动态[J].农药,2006,45(8):552-553.
[10]郝金芝.高效液相色谱法测定水果中的多菌灵[J].中国卫生检验杂志,2004,14(5):586-587.
[11]中华人民共和国农业部.蔬菜及水果中多菌灵等16种农药残留测定液相色谱-质谱-质谱联用法:NY/T 1453-2007[S].北京:中国标准出版社,2007.
[12]洪月玲,钟化舰,董小海.LC-MS/MS法测定水果、蔬菜中多菌灵残留的研究[J].河南预防医学杂志,2008,19(1):19-21.
[13]蔡世炎,游文玮,李耀群.导数同步荧光法快速检测香菇中的多菌灵[J].分析测试学报,2007,26(1):117-119.