色谱

色谱 ›› 2012, Vol. 30 ›› Issue (09): 962-965.DOI: 10.3724/SP.J.1123.2012.06008

• 技术与应用 • 上一篇    下一篇

液相色谱-串联质谱法测定蔬菜和水果中硝苯菌酯的残留量

张志勇1, 单炜力2, 简秋2, 段丽芳2, 沈燕1, 刘贤金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:2012-06-06 修回日期:2012-07-07 出版日期:2012-09-28 发布日期:2012-09-20
  • 通讯作者: 刘贤金,博士,研究员,主要从事农产品安全性研究. E-mail: jaasliu@jaas.ac.cn.
  • 基金资助:

    江苏省农业科技自主创新资金项目(CX(11)4069).

Determination of meptyldinocap residues in vegetable and fruit by liquid chromatography-tandem mass spectrometry

ZHANG Zhiyong1, SHAN Weili2, JIAN Qiu2, DUAN Lifang2, 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:2012-06-06 Revised:2012-07-07 Online:2012-09-28 Published:2012-09-20

PDF

481

被引次数

8

摘要： 建立了一种通过检测硝苯菌酯(2,4-dinitro-6-(1-methylheptyl) phenyl crotonate, 2,4-DNOPC)相应的水解产物2,4-二硝基-6-(1-甲基庚基)苯酚(2,4-dinitro-6-(1-methylheptyl) phenol, 2,4-DNOP)来测定蔬菜和水果中2,4-DNOPC残留量的液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)检测方法。蔬菜和水果样品用丙酮-甲醇-盐酸的混合液进行液-液分配提取,在碱性条件下超声水解后再进行液-液分配提取,然后进行LC-MS/MS测定。2,4-DNOPC在6种蔬菜和水果中的回收率试验结果表明,2,4-DNOPC在甘蓝中的添加回收率为89.7%～93.3%,相对标准偏差(RSD)为6.3%～8.5%;在黄瓜中的添加回收率为87.7%～95.1%, RSD为5.8%～10.4%;在番茄中的添加回收率为89.3%～96.0%, RSD为6.8%～9.2%;在苹果中的添加回收率为92.0%～98.3%, RSD为5.1%～10.3%;在梨中的添加回收率为89.0%～95.0%, RSD为5.3%～10.2%;在葡萄中的添加回收率为81.2%～95.8%, RSD为5.8%～10.4%。2,4-DNOPC在6种蔬菜和水果的最低检测浓度均为0.01 mg/kg。该检测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,适用于蔬菜和水果中硝苯菌酯残留量的检测。

关键词: 蔬菜, 水果, 硝苯菌酯, 液相色谱-串联质谱

Abstract: A method was developed for the determination of the residues of meptyldinocap (2,4-dinitro-6-(1-methylheptyl) phenyl crotonate, 2,4-DNOPC) as 2,4-dinitrooctylphenol (2,4-dinitro-6-(1-methylheptyl) phenol, 2,4-DNOP), which is a hydrolysate of 2,4-DNOPC, in six vegetable and fruit by using liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). The residues of 2,4-DNOPC in vegetable and fruit samples were extracted by the mixture of acetone, methanol and hydrochloric acid, then extracted by liquid-liquid partitioning, hydrolyzed under alkaline condition with ultrasonication, and extracted again by liquid-liquid partitioning, then analyzed by using LC-MS/MS in multiple reaction monitoring (MRM) mode via negative electrospray ionization with an Agilent ZORBAX SB-C18 column. The method was validated at four fortification levels in vegetable and fruit. The validation results were as follows: the recoveries of 2,4-DNOPC in cabbages were from 89.7% to 93.3% (the relative standard deviations (RSD) of 6.3%~8.5%), in cucumbers from 87.7% to 95.1% (RSD of 5.8%~10.4%), in tomatoes from 89.3% to 96.0% (RSD of 6.8%~9.2%), in apples from 92.0% to 98.3% (RSD of 5.1%~10.3%), in pears from 89.0% to 95.0% (RSD of 5.3%~10.2%), in grapes from 81.2% to 95.8% (RSD of 5.8%~10.4%). The limits of quantification of 2,4-DNOPC in all the test samples were 0.01 mg/kg. The results showed that the method is simple, rapid, and is characterized with acceptable sensitivity and accuracy to meet the requirements of the pesticide residue analysis. This method is applicable to confirm the residues of meptyldinocap in vegetable and fruit samples.

Key words: fruit, meptyldinocap, vegetable, liquid chromatography-tandem mass spectrometry (LC-MS/MS)