氣相色譜/串聯(lián)質(zhì)譜法測定芒果中的腈苯唑和溴螨酯殘留

李萍萍 程景 黎舒懷 李春麗

摘 要 建立了氣相色譜/三重串聯(lián)四級桿質(zhì)譜分析芒果中腈苯唑和溴螨酯農(nóng)藥殘留的方法。采用乙腈提取，Carbon/NH2固相萃取小柱凈化后采用氣相色譜/三重串聯(lián)四級桿質(zhì)譜多反應(yīng)（MRM）模式下進行外標(biāo)法定量測定，并對腈苯唑和溴螨酯的基質(zhì)效應(yīng)進行分析。結(jié)果表明：2種農(nóng)藥在0.01～1.00 mg/L范圍內(nèi)線性關(guān)系均良好。該方法對腈苯唑和溴螨酯的檢出限（LOD）分別為0.003、0.002 mg/kg，定量限（LOQ）分別為0.010、0.008 mg/kg。在0.01～0.05 mg/kg濃度添加水平下，2種農(nóng)藥的平均回收率處于76.5%～89.6%之間，相對標(biāo)準(zhǔn)偏差（RSD）不大于10.3%。該方法背景干擾少，靈敏度高，重復(fù)穩(wěn)定性好，可用于分析芒果中腈苯唑和溴螨酯的殘留測定。

關(guān)鍵詞 氣相色譜-串聯(lián)質(zhì)譜；農(nóng)藥殘留；腈苯唑；溴螨酯；芒果

中圖分類號 S667.8 文獻(xiàn)標(biāo)識碼 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