色谱

色谱 ›› 2012, Vol. 30 ›› Issue (01): 91-94.DOI: 10.3724/SP.J.1123.2011.07014

• 技术与应用 • 上一篇    下一篇

QuEChERS-高效液相色谱-串联质谱法测定黄瓜和土壤中甲基硫菌灵和多菌灵

张志勇1, 龚勇2, 单炜力2, 简秋2, 沈燕1, 刘贤进1*   

  1. 1. 江苏省食品质量安全重点实验室 农业部食品安全监控重点开放实验室, 江苏 南京 210014; 2. 农业部农药检定所, 北京 100125
  • 收稿日期:2011-07-07 修回日期:2011-08-18 出版日期:2012-01-28 发布日期:2012-03-01
  • 通讯作者: 刘贤进,博士,研究员,主要从事农产品安全性研究
  • 基金资助:

    江苏省农业科技自主创新基金项目(CX(11)4069).

Determination of thiophanate-methyl and carbendazim in cucumber and soil by QuEChERS-high performance liquid chromatography-triple quadrupole tandem mass spectrometry

ZHANG Zhiyong1, GONG Yong2, SHAN Weili2, JIAN Qiu2, SHEN Yan1, LIU Xianjin1*   

  1. 1. Key Laboratory of Food Safety and Quality of Jiangsu Province, Key Laboratory of Food Safety Monitoring and Management of Ministry of Agriculture, Nanjing 210014, China; 2. Institute for the Control of Agrochemicals, Ministry of Agriculture, Beijing 100125, China
  • Received:2011-07-07 Revised:2011-08-18 Online:2012-01-28 Published:2012-03-01

PDF

567

被引次数

85

摘要： 建立了黄瓜和土壤样品中甲基硫菌灵和多菌灵的QuEChERS-高效液相色谱-电喷雾串联质谱(HPLC-ESI-MS/MS)检测方法。样品用乙腈溶液提取,经QuEChERS方法净化,以Agilent ZORBAX SB-C18色谱柱(30 mm×2.1 mm, 5 μm)进行HPLC分离,以电喷雾电离串联质谱正离子多反应监测(MRM)模式进行测定。对甲基硫菌灵和多菌灵在黄瓜和土壤中4个添加水平(0.01、0.05、0.1和1.0 mg/kg)下的回收率进行了测定,甲基硫菌灵在黄瓜中的添加回收率为87.3%～96.0%(相对标准偏差(RSD)为8.0%～9.3%),在土壤中的添加回收率为88.8%～93.4%(RSD为5.3%～9.9%);多菌灵在黄瓜中的添加回收率为87.1%～92.3%(RSD为5.2%～7.5%),在土壤中的添加回收率为85.8%～90.9%(RSD为5.3%～13.2%)。该方法样品前处理简单、快速,分析时间短,灵敏度、准确度和精密度均符合农药残留检测要求,适用于黄瓜和土壤中甲基硫菌灵和多菌灵残留的检测。

关键词: QuEChERS, 多菌灵, 高效液相色谱-串联质谱, 黄瓜, 甲基硫菌灵, 土壤

Abstract: A method was developed for the determination of thiophanate-methyl and carbendazim residues in cucumber and soil by using QuEChERS-high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS). The residues in the samples were extracted by acetonitrile, cleaned up by developed QuEChERS method, and then analyzed by using LC-MS/MS in multiple reaction monitoring (MRM) mode via positive electrospray ionization with an Agilent ZORBAX SB-C18 column (30 mm×2.1 mm, 5 μm) as the analytical column. The recoveries of thiophanate-methyl spiked at four levels of 0.01, 0.05, 0.1 and 1.0 mg/kg were from 87.3% to 96.0% with the relative standard deviations (RSDs) of 8.0%~9.3% in cucumber, from 88.8% to 93.4% with the RSDs of 5.3%~9.9% in soil; the recoveries of carbendazim spiked at the same levels as those of thiophanate-methyl were from 87.1% to 92.3% with the RSDs of 5.2%~7.5% in cucumber, from 85.8% to 90.9% with the RSDs of 5.3%~13.2% in soil. The method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements of the pesticide residue analysis. This method is applicable to confirm the residues of thiophanate-methyl and carbendazim in cucumber and soil.

Key words: carbendazim, cucumber, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), soil, thiophanate-methyl, QuEChERS