QuEChERS-超高效液相色谱法-串联质谱法同时检测猪组织中赛庚啶及可乐定残留量

Simulaneous Determination of Cyproheptadine and Clonidine in Pig Issues by QuEChERS and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

建立了Qu ECh ERS前处理结合超高效液相色谱-串联质谱同时检测猪组织中赛庚啶和可乐定残留量的方法。猪肉样品添加0.5 g C18粉,猪肝和猪肾样品添加3.0 g硫酸镁和2.0 g氯化钠,再分别加入10 m L 0.1%甲酸乙腈进行提取,提取液经浓缩后采用LC-MS/MS进行检测,内标法定量。该方法线性关系良好,猪肉、猪肝和猪肾中赛庚啶和可乐定在1~50μg/kg浓度范围内加标回收率分别为62%~112%和106%~121%,相对标准偏差均<10%,方法检出限为0.5μg/kg。方法灵敏度高,选择性好,可作为猪组织中赛庚啶和可乐定残留量检测的确证方法。

A method has been developed for the simultaneous determination of the cyproheptadine and clonidine residuals in pig issues using QuEChERS method coupled with ultra performance liquid chromatography - tandem mass spectrometry （ UPLC - MS/MS）. The drugs were extracted with sufficiently acidic acetonitrile. Anhydrous magnesium sulfate and anhydrous sodium chloride were used for the salting -out process. C18 powder was used for the clean-up process. The drugs were analyzed by UPLC -MS/MS in multiple reaction monitoring（MRM） mode via electrospray ionization. Cyproheptadine and clonidine were quantified by internal standard method. The calibration curves of the drugs were linear in the range of 0.5 -100 ng/mL with the correlation coefficients more than 0.99. The LOD of cyproheptadine and clonidine in pig issues were 0.5 μ/kg. Add in the blank pig issues 1 -50 μg/kg level, an average recovery of 62% - 112% for cyproheptadine, and 106% - 121% for clonidine with the relative standard deviation was 〈 10%. The method is simple, rapid and high recovery and good reproducibility for quantitative and confirmatory analysis in cyproheptadine and clonidine residues