高效液相色谱-串联质谱法快速测定甘蔗中杀虫双残留量

doi:10.7506/spkx1002-6630-201516043

食品科学

高效液相色谱-串联质谱法快速测定甘蔗中杀虫双残留量

黄健祥，路大海，丁晨红，寥若昕，王富华*

广东省农业科学院农产品公共监测中心，农业部农产品质量安全检测与评价重点实验室，
农业部农产品质量安全风险评估实验室（广州），广东广州 510640

出版日期:2015-08-25 发布日期:2015-08-17
通讯作者: 王富华
基金资助:
国家自然科学基金青年科学基金项目（21305019）；公益性行业（农业）科研专项（201303088）；
广东省农业科学院院长基金项目（201218）

Fast Detection of Bisultap Residue in Sugarcane by Liquid Chromatography-Tandem Mass Spectrometry

HUANG Jianxiang, LU Dahai, DING Chenhong, LIAO Ruoxin, WANG Fuhua*

Laboratory of Quality and Safety Risk Assessment for Agro-product (Guangzhou), Ministry of Agriculture, Key Laboratory of
Testing and Evaluation for Agro-product Quality and Safety, Ministry of Agriculture, Public Monitoring Center for Agro-product,
Guangdong Academy of Agricultural Sciences, Guangzhou 510640, China

Online:2015-08-25 Published:2015-08-17
Contact: WANG Fuhua

摘要/Abstract

摘要：

建立了一种简便、快速、灵敏、准确的甘蔗中杀虫双的液相色谱-串联质谱分析方法。优化了色谱、质谱条件和提取溶剂的组成，以甲醇-水（50∶50，V/V）提取样品中的杀虫双，离心后上层清液过滤后直接上机检测，无需进一步净化。甘蔗中杀虫双的检出限为1.0 μg/kg，定量限为4.0 μg/kg。甘蔗中5 个添加量4.0、10、100、200 μg/kg和500 μg/kg的回收率为62.3%～108.4%，相对标准偏差为5.1%～14.8%。采用本方法分析了8 例广州市场上的甘蔗样品，均未检出杀虫双。

关键词: 杀虫双, 甘蔗, 液相色谱-串联质谱

Abstract:

In this study, a simple, fast, sensitive and accurate liquid chromatography-tandem mass spectrometry (LC-MS-MS)
method was developed for the analysis of bisultap in sugarcane. The chromatographic conditions, the mass spectrometry
parameters and the composition of extraction solvent were optimized. Bisultap was extracted with 50% methanol-water
(50:50, V/V). Then, the extraction phase was filtered after centrifugation, followed by LC-MS-MS detection without further
purification. The limit of detection for bisultap in sugarcane was 1.0 μg/kg and the limit of quantification was 4.0 μg/kg.
Recoveries at five spiked levels of 4.0, 10, 100, 200 and 500 μg/kg ranged from 62.3% to 108.4% with relative standard
deviations of 5.1% to 14.8%. The proposed method was applied to the analysis of eight sugarcane samples from local
markets in Guangzhou and no bisultap was detected.

Key words: bisultap, sugarcane, liquid chromatography-tandem mass spectrometry

中图分类号:

O657.72

黄健祥，路大海，丁晨红，寥若昕，王富华. 高效液相色谱-串联质谱法快速测定甘蔗中杀虫双残留量[J]. 食品科学, doi: 10.7506/spkx1002-6630-201516043.

HUANG Jianxiang, LU Dahai, DING Chenhong, LIAO Ruoxin, WANG Fuhua. Fast Detection of Bisultap Residue in Sugarcane by Liquid Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, doi: 10.7506/spkx1002-6630-201516043.

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高效液相色谱-串联质谱法快速测定甘蔗中杀虫双残留量

Fast Detection of Bisultap Residue in Sugarcane by Liquid Chromatography-Tandem Mass Spectrometry

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