猪肉中盐酸克伦特罗和盐酸莱克多巴胺残留量检测气质联用法探讨

Determination of Clenbuterol Hydrochloride and Ractopamine Hydrochloride Residual in Pork Tissues Gas Chromatography/mass Spectrometry Discussion

根据贵阳市农产品质量安全监督检验测试中心试验室检测技术水平,对气相色谱-质谱测定猪肉中盐酸克伦特罗、盐酸莱克多巴胺残留量的方法进行了探讨。试样用甲醇提取和离子交换固相萃取柱净化,氮气吹干,用衍生化试剂99%双三甲基硅基三氟乙酰胺(BSTFA)+1%三甲基氯硅烷(TMCS)进行衍生,用正己烷定容,于气相色谱-质谱仪上进行测定。结果表明:盐酸克伦特罗和盐酸莱克多巴胺在5～500 ng/ml范围内均有很好的线性关系。试样中盐酸克伦特罗的平均回收率为95.40%～99.94%,相对标准偏差(RSD)≤3.55%;盐酸莱克多巴胺的平均回收率为96.60%～99.96%,相对标准偏差(RSD)≤3.35%。该方法检测限为盐酸克伦特罗和盐酸莱克多巴胺均为0.5μg/kg。

According to the technical level of the laboratory testing of gas chromatography - mass spectrometry determination of clenbuterol in pork ,ractopamine hydrochloride residue methods are discussed. Samples extracted with methanol and ion - exchange solid phase extraction cartridge, evaporated to dryness,derivatization reagent with 99% of double - trimethylsilyl trifluoroacetamide （BSTFA） ＋ 1% trimethylchlorosilane （TMCS） were derived, using hexane to volume, the gas chromatography - mass spectrometer were determined. The results showed that clenbuterol and ractopamine hydrochloride in the range of 5 - 500 ng/ml have a good linear relationship. Clenbuterol in the sample, the average recovery was 95.40% - 99.94%, relative standard deviation （ RSD ） ≤ 3.55% ; ractopamine hydrochloride, the average recovery was 96.60% - 99.96% , relative standard deviation （RSD） ≤ 3.35 %. The method detection limit of clenbuterol and ractopamine hydrochloride are 0. 5μg/kg.