液相色谱-串联质谱法测定花生中丙硫菌唑及其脱硫代谢物

建立了液相色谱-串联质谱(HPLC-MS/MS)同时检测花生中丙硫菌唑及其主要代谢物硫酮菌唑的方法.花生样品经乙腈提取后,用乙腈饱和的正己烷除掉脂类杂质,C18分散固相萃取净化样品.采用含有5 mmol/L乙酸铵、0.2％乙酸和乙腈作为流动相进行梯度洗脱,在电喷雾-多反应监测离子模式下进行定性与定量分析.丙硫菌唑和硫酮菌唑在2.0,4.0和20.0 μg/kg的添加浓度时回收率为87.22％～102.46％；相对标准偏差小于10.0％；方法定量限为2.0 μg/kg.

Determination of Prothioconazole and Prothioconazole-desthio in Peanut Samples by Liquid Chromatography-Tandem Mass Spectrometry

A sensitive method was developed for determination of prothioconazole and prothioconazole-desthio in peanut.The analytes were extracted from the peanut samples by acetonitril,and defatted with n-hexane saturated by acetonitrile.Then the samples were purified by dispersion solid phase extraction using ODS C18 sorbent,and analyzed by liquid chromatography tandem mass spectrometry(LC-MS/MS).Prothioconazole and prothioconazole-desthio were separated on a reversed phase column using a gradient elution program of aqueous solution containing 5 mmol/L ammonium acetate and 0.2% acetic acid(A) and acetonitrile solution(B).Analyte confirmation was performed using multiple reaction monitoring(MRM) with one precursor ion and two productions as identifiers.The recoveries were in the range of 87.2%-102.46%,and the relative standard deviation(RSDs) were less than 9.97% at 2.0,4.0,and 20.0 μg/kg three spiked levels for prothioconazole and prothioconazole-desthio.The limits of quantification(LOQ) for the two analytes were 2.0 μg/kg.