超高效液相色谱-串联质谱法测定热带水果中杀虫双残留

doi:10.3724/SP.J.1123.2018.08018

色谱 ›› 2018, Vol. 36 ›› Issue (12): 1223-1227.DOI: 10.3724/SP.J.1123.2018.08018

超高效液相色谱-串联质谱法测定热带水果中杀虫双残留

林涛^1,2, 邵金良¹, 刘兴勇¹, 王静³, 邹艳虹¹, 李茂萱¹, 刘宏程^1,2

1. 云南省农业科学院质量标准与检测技术研究所, 云南昆明 650205;
2. 农业农村部农产品质量安全风险评估实验室(昆明), 云南昆明 650205;
3. 云南省保山市龙陵县农产品质量安全检验检测站, 云南龙陵 678300

收稿日期:2018-08-14 出版日期:2018-12-08 发布日期:2014-11-06
通讯作者: 刘宏程,Tel:(0871)65140430,E-mail:liuorg@163.com
基金资助:
国家农产品质量安全风险评估项目（GJFP201800402）；云南省科技厅重大专项计划（2018BC005-04）；云南省科技创新平台建设计划项目（2014DA001）.

Determination of bisultap residue in tropical fruits by ultra performance liquid chromatography-tandem mass spectrometry

LIN Tao^1,2, SHAO Jinliang¹, LIU Xingyong¹, WANG Jing³, ZOU Yanhong¹, LI Maoxuan¹, LIU Hongcheng^1,2

1. Institute of Quality Standards & Testing Technique, Yunnan Academy of Agricultural Science, Kunming 650205, China;
2. Laboratory of Quality & Safety Risk Assessment for Agro-Products(Kunming), Ministry of Agriculture and Rural Affairs, Kunming 650205, China;
3. Agricultural Products Quality and Safety Inspection and Testing Station of Longling County, Baoshan City, Yunnan Province, Longling 678300, China

Received:2018-08-14 Online:2018-12-08 Published:2014-11-06
Supported by:
National Agricultural Product Quality and Safety Risk Assessment Project (No. GJFP201800402); Major Special Project of Yunnan Science and Technology Department (No. 2018BC005-04); Yunnan Science and Technology Innovation Platform Construction Project (No. 2014DA001).

摘要/Abstract

摘要：

采用改进的QuEChERS方法，结合超高效液相色谱-串联质谱法（UPLC-MS/MS），建立了热带水果中杀虫双残留的测定方法。热带水果经含1%（v/v）乙酸的乙腈溶液二次提取，200 mg N-丙基乙二胺（PSA）、100 mg C18、300 mg MgSO₄和500 mg柠檬酸氢二钠净化。采用CAPCELL CORE PC亲水色谱柱进行分离，在负离子多反应监测（MRM）模式下检测，外标法定量。结果表明，杀虫双在0.1~10.0 μg/L范围内线性关系良好，相关系数（r²）为0.9993，检出限和定量限分别为0.015 μg/kg和0.05 μg/kg，加标回收率为81.0%~88.3%，相对标准偏差（RSD）为3.9%~6.2%。该法净化效果好，灵敏度高，适于热带水果中杀虫双残留的快速定性和定量分析。

关键词: 残留, 超高效液相色谱-串联质谱, 热带水果, 杀虫双

Abstract:

A method for the determination of bisultap in tropical fruits was developed by modified QuEChERS method and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The tropical fruit samples were twice extracted with acetonitrile containing 1% (v/v) acetic acid, and purified by 200 mg of primary secondary amine (PSA), 100 mg of C18, 300 mg of MgSO₄ and 500 mg of disodium hydrogen citrate. The analyte was separated on a CAPCELL CORE PC hydrophilic column, detected in the negative ion multiple reaction monitoring (MRM) mode, and quantified by external standard method. A good linear relationship in the range of 0.1-10.0 μg/L was obtained with the correlation coefficient (r²) of 0.9993. The limit of detection and limit of quantification were 0.015 μg/kg and 0.05 μg/kg, respectively. The spiked recoveries were in the range of 81.0%-88.3% with the relative standard deviations from 3.9% to 6.2%. The method has good purification effect and high sensitivity, and is suitable for the rapid analysis of the bisultap residues in tropical fruits.

Key words: bisultap, residues, tropical fruit, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

中图分类号:

O658

林涛, 邵金良, 刘兴勇, 王静, 邹艳虹, 李茂萱, 刘宏程. 超高效液相色谱-串联质谱法测定热带水果中杀虫双残留[J]. 色谱, 2018, 36(12): 1223-1227.

LIN Tao, SHAO Jinliang, LIU Xingyong, WANG Jing, ZOU Yanhong, LI Maoxuan, LIU Hongcheng. Determination of bisultap residue in tropical fruits by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(12): 1223-1227.

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超高效液相色谱-串联质谱法测定热带水果中杀虫双残留

Determination of bisultap residue in tropical fruits by ultra performance liquid chromatography-tandem mass spectrometry

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