| 摘要: |
| 建立了QuEChERS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 mL 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1～50 μg/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0.5 μg/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。 |
| 关键词: 赛庚啶 可乐定 液相色谱-串联质谱 猪组织 |
| DOI： |
| 投稿时间：2016-08-26修订日期：2016-09-29 |
| 基金项目:上海市科技兴农重点攻关项目 ［沪农科攻字（2014）第3-3号］；国家公益性行业（农业）科研专项（201203023） |
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| Simulaneous Determination of Cyproheptadine and Clonidine in Pig Issues by QuEChERS and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry |
|
| (Shanghai Animal Disease Control Center) |
| Abstract: |
| 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 μg/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. |
| Key words: cyproheptadine clonidine LC/MS/MS pig issues |
