气相色谱/串联质谱法测定芒果中的腈苯唑和溴螨酯残留

李萍萍 程景 黎舒怀 李春丽

摘 要 建立了氣相色谱/三重串联四级杆质谱分析芒果中腈苯唑和溴螨酯农药残留的方法。采用乙腈提取，Carbon/NH2固相萃取小柱净化后采用气相色谱/三重串联四级杆质谱多反应（MRM）模式下进行外标法定量测定，并对腈苯唑和溴螨酯的基质效应进行分析。结果表明：2种农药在0.01～1.00 mg/L范围内线性关系均良好。该方法对腈苯唑和溴螨酯的检出限（LOD）分别为0.003、0.002 mg/kg，定量限（LOQ）分别为0.010、0.008 mg/kg。在0.01～0.05 mg/kg浓度添加水平下，2种农药的平均回收率处于76.5%～89.6%之间，相对标准偏差（RSD）不大于10.3%。该方法背景干扰少，灵敏度高，重复稳定性好，可用于分析芒果中腈苯唑和溴螨酯的残留测定。

关键词 气相色谱-串联质谱；农药残留；腈苯唑；溴螨酯；芒果

中图分类号 S667.8 文献标识码 A

Determination of Fenbuconazole and Bromopropylate Pesticide

Residues in Mango Using Gas Chromatography-triple

Quadrupole Mass Spectrometry

LI Pingping1 *， CHENG Jing2， LI Shuhuai1， LI Chunli1

1 Analytical and Test Center， Chinese Academy of Tropical Agricultural Sciences， Haikou， Hainan 571101， China

2 Quality Inspection and Test Center for Agricultural Products of Heilongjiang Province， Harbin， Heilongjiang 150090， China

Abstract A method was developed for the determination of fenbuconazole and bromopropylate pesticide residues in mango using gas chromatography-triple quadrupole mass spectrometry（GC-MS/MS）. The pesticides were extracted with acetonitrile， and then purified by the column of Carbon/NH2. The extracts were determined by the mode of multiple reaction monitoring（MRM）of GC-MS/MS using external standard method and the matrix effect was investigated. The results showed that the linearity range of the method between 0.01 mg/L and 1.00 mg/L was fine. The limits of determination of the method were 0.003 mg/kg for fenbuconazole and 0.002 mg/kg for bromopropylate. The limits of quantitation（LOQ）were 0.01 mg/kg for fenbuconazole and 0.008 mg/kg for bromopropylate. The recoveries of all pesticedes at the spiked level of 0.010 mg/kg to 0.05 mg/kg into mango matrixes were in the range of 76.5% to 89.6%，and the relative standard deviations（RSDs）were less than 10.3%. It is proved that the method is stable，sensitive，and good reproducible with low background，therefore it can be used in the analysis of fenbuconazole and bromopropylate pesticide residues in mango.

Key words Gas chromatography-triple quadrupole mass spectrometry（GC-MS/MS）； Pesticide residues； Fenbuconazole； Bromopropylate； Mango

doi 10.3969/j.issn.1000-2561.2015.04.027