液相色谱-串联质谱法测定果蔬中双三氟虫脲、四氯虫酰胺和氰虫酰胺残留

引用本文: 崔淑华, 李瑞娟, 张晓梅, 程刚, 王宇, 李正义. 液相色谱-串联质谱法测定果蔬中双三氟虫脲、四氯虫酰胺和氰虫酰胺残留[J]. 分析化学, 2017, 45(4): 545-552. doi: 10.11895/j.issn.0253-3820.160493 shu

Citation: CUI Shu-Hua, LI Rui-Juan, ZHANG Xiao-Mei, CHENG Gang, WANG Yu, LI Zheng-Yi. Determination of New Bistrifluron, Cyantraniliprole and SYP9080 Residues in Fruits and Vegetables by Liquid Chromatography- Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2017, 45(4): 545-552. doi: 10.11895/j.issn.0253-3820.160493 shu

液相色谱-串联质谱法测定果蔬中双三氟虫脲、四氯虫酰胺和氰虫酰胺残留

崔淑华 ^1, ,
李瑞娟 ^2, ,
张晓梅 ^1, ,
程刚 ^1, ,
王宇 ^1, ,
李正义 ^1,

1.
山东出入境检验检疫局检验检疫技术中心, 青岛 266002;
2.
山东省农业科学院植物保护研究所, 济南 250100
基金项目:
本文系山东出入境检验检疫科研项目（No.SK201425）资助

摘要: 建立了蔬菜和水果中双三氟虫脲、四氯虫酰胺和氰虫酰胺3种新型杀虫剂的分散固相萃取-液相色谱-串联质谱检测方法。样品经乙腈均质提取，混合使用乙二胺-N-丙基硅烷（PSA）和C₁₈基质分散净化剂进行净化，液相色谱-三重四极杆串联质谱（LC-MS/MS）同时进行检测。双三氟虫脲和四氯虫酰胺采用多反应监测负离子模式，氰虫酰胺采用多反应监测正离子模式。双三氟虫脲在苹果、洋葱和经微波处理的洋葱样品中均不存在基质效应，可采用纯溶剂标准外标法或者采用基质匹配标准溶液定量检测；四氯虫酰胺和氰虫酰胺存在程度不同的基质减弱效应，采用空白基质匹配的校正标准曲线外标法定量。3种杀虫剂均在0.2-100 μg/L线性范围内具有良好的线性关系，相关系数均大于0.9990。在0.005-2.000 mg/kg范围内，平均添加回收率为81.6%-99.9%，相对标准偏差为3.6%-9.8%。氰虫酰胺、四氯虫酰胺和双三氟虫脲的检出限分别为0.064，0.048和0.001 μg/kg，定量限分别为0.210，0.160和0.004 μg/kg。

关键词:

English

Determination of New Bistrifluron, Cyantraniliprole and SYP9080 Residues in Fruits and Vegetables by Liquid Chromatography- Tandem Mass Spectrometry

1.
Inspection and Quarantine Technology Center of Shandong Exit/Entry Inspection and Quarantine Bureau, Qingdao 266002, China;
2.
Institute of Plant Protection, Shandong Academy of Agriculture, Jinan 250100, China
Received Date: 29 June 2016
Revised Date: 04 January 2017

Abstract: A liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed for the determination of bistrifluron, cyantraniliprole and SYP9080 residues in fruits and vegetables. The analytes were extracted from samples with acetonitrile, and purified by dispersion solid phase extraction using C18 and primary secondary amine (PSA) as solid phase adsorbent, then analyzed by LC-MS/MS. Bistrifluron and SYP9080 were analyzed with negative ion multiple-reaction monitoring (MRM), cyantraniliprole was analyzed with positive ion MRM. The matrix-induced weakening effect was observed in the analysis of cyantraniliprole and SYP9080 in several samples including cucumber, apple and onion, and the weakening extent of the matrix-induced effect depended on the sample properties. But no matrix effect was found in the analysis of bistrifluron in several samples. The interference of matrix was reduced by using the matrix-matched calibration standards curve in the analysis of cyantraniliprole and SYP9080. Bistrifluron could be quantified by an external standard of the matrix-matched calibration standards or the pure solvent calibration standards. The linear range was from 0.2 μg/L to 100 μg/L for bistrifluron, cyantraniliprole and SYP9080 with the good correlation coefficients (r≥0.9990). The recoveries of cucumber, grape, apple and scallion added bistrifluron at 0.005-2 mg/kg were 79.8%-99.9%, with relative standard deviations (RSD) of 3.6%-9.8%. The limits of quantification (S/N=10) were 0.210 μg/kg, 0.160 μg/kg and 0.004 μg/kg, and limits of detection (S/N=3) were 0.064 μg/kg, 0.048 μg/kg and 0.001 μg/kg for bistrifluron, cyantraniliprole and SYP9080, respectively.

Key words:

Liquid chromatography-tandem mass spectrometry
/ Fruits and vegetables
/ Residues
/ Bistrifluron
/ SYP9080

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沈阳化工大学材料科学与工程学院沈阳 110142

液相色谱-串联质谱法测定果蔬中双三氟虫脲、四氯虫酰胺和氰虫酰胺残留

English

Determination of New Bistrifluron, Cyantraniliprole and SYP9080 Residues in Fruits and Vegetables by Liquid Chromatography- Tandem Mass Spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

液相色谱-串联质谱法测定果蔬中双三氟虫脲、四氯虫酰胺和氰虫酰胺残留

English

Determination of New Bistrifluron, Cyantraniliprole and SYP9080 Residues in Fruits and Vegetables by Liquid Chromatography- Tandem Mass Spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs