UPLC-MS/MS法测定蔬菜中代森锰锌和甲基代森锌

Determination of mancozeb and propineb in vegetables with UPLC-MS/MS

建立了蔬菜中的代森锰锌和甲基代森锌经碘甲烷衍生化反应后用正己烷液液萃取,并利用UPLC-MS/MS检测的方法。实验优化了衍生化的条件和提取方法,以外标法定量分析。方法具有良好的线性关系,代森锰锌和甲基代森锌质量浓度分别在6.89~344.5 ng/mL与6.15~307.5 ng/mL范围内线性回归系数r均大于0.995;检测限均小于1μg/kg;代森锰锌和甲基代森锌在蔬菜中的加标回收率在83.1%~97.6%范围内,相对标准偏差(RSD,n=6)在4.3%~13%范围内。方法可满足对蔬菜中的代森锰锌及甲基代森锌农药残留检测的要求。

A sensitivity and reproducibility method was developed for the determination of the mancozeb and propineb pesticides in vegetables by ultra high performance liquid chromatographytandem quadrupole mass spectrometry（ UPLC-MS/MS）. The samples were derived with methyl iodide and then extracted by hexane for liquid – liquid extraction. The conditions of derivatization and the extraction method were optimized and the quantitative analysis of external standard method were carried out. The method has a good linear relationship and the linear regression coefficients were greater than0. 995. The linear ranges of mancozeb and propineb in vegetable were 6. 89 to 344. 5 ng/mL and 6. 15 to 307. 5 ng/mL,respectively. And the limits of detection were less than 1 μg/kg. The recoveries of mancozeb and propineb were ranged from 83. 1% to 97. 6% and the relative standard deviations（ RSD,n = 6） in the range of 4. 3% - 13%. This method can effectively satisfy the requirements for residue detection of mancozeb and propineb pesticides in vegetables.