UPLC-MS/MS测定生乳与豆制饮品中咪唑烟酸残留

该研究考察生乳与豆制饮品中咪唑烟酸的前处理条件，旨在建立一种超高效液相色谱-串联质谱（UPLC-MS/MS）检测生乳与豆制饮品中咪唑烟酸农药残留的方法。结果表明，该方法的前处理条件为采用甲酸∶乙腈=5∶995(V/V)提取，HLB固相萃取柱净化，20%乙腈水溶液定容。选择电喷雾离子源正离子（ESI+）多反应监测（MRM）模式，采用UPLC-MS/MS测定咪唑烟酸，外标法定量。在此条件下，咪唑烟酸在2.0～30.0μg/L质量浓度范围内线性关系良好，相关系数R2>0.99，生乳和豆制饮品中咪唑烟酸的检出限（LOD）和定量限（LOQ）均分别为0.002 mg/kg、0.005 mg/kg，加标回收率为80.77%～90.35%，精密度试验结果的相对标准偏差（RSD）为1.43%～5.27%，说明该方法简便、快速、准确，具有一定的推广价值，可用于生乳与豆制饮品中咪唑烟酸残留量检测。

Determination of imazapyr residues in raw milk and soybean drinks by UPLC-MS/MS

The pretreatment conditions of imazapyr in raw milk and soybean drinks were studied, aiming to establish a method for the detection of imazapyr residues in raw milk and soybean drinks by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The results showed that the pretreatment conditions of the method were as follows: extraction with formic acid: acetonitrile = 5∶995 (V/V), purification with HLB solid phase extraction column, constant volume with 20% acetonitrile water solution. Selecting electrospray ionization positive ion (ESI+) multiple reaction monitoring (MRM) mode, the imazapyr was determined by UPLC-MS/MS and quantified by external standard method. Under these conditions, the imazapyr had a good linear relationship in the concentration range of 2.0-30.0 μg/L with correlation coefficient R2＞0.99, the limit of detection (LOD) and the limit of quantitation (LOQ) of imazapyr in raw milk and soy drinks were both 0.002 mg/kg and 0.005 mg/kg, respectively, the standard recovery rate was 80.77%-90.35%, and the relative standard deviation (RSD) of precision test results was 1.43%-5.27%, indicating that the method was simple, rapid and accurate, with certain popularization value, and could be used for the determination of imazapyr residues in raw milk and soybean drinks.