液相色谱-串联质谱法同时测定饲料中矮壮素和缩节胺的残留

本文采用高效液相色谱-串联质谱(HPLC-MS/MS)同时测定饲料中的矮壮素和缩节胺残留。样品先用正己烷脱除油脂,后用缓冲溶液(含0.2%甲酸-0.05mol/L乙酸铵)提取,离心上清液用乙腈沉淀净化后进行测试。结果表明:两种化合物在1.0~50.0μg/L范围内线性关系良好;定量限(S/N=10)矮壮素为0.32μg/L,缩节胺为0.45μg/L;加标回收率为91.7%~94.3%;相对标准偏差3.9%~6.1%;实测有30%的样品中含有矮壮素或缩节胺,含量范围为:矮壮素11.2μg/kg-78.4μg/kg;缩节胺9.7μg/kg-126.6μg/kg。该方法简便、快速、灵敏和准确,适合饲料中这两种农药残留的快速检测和定量分析。

Determination of chlormequat and mepiquat chloride residues in forage using high performance liquid chromatography-tandem mass spectrometry

This paper established the methods of ehlormequat and mepiquat chloride residual of forage simultaneous were determined with high performance liquid chromatography-tandem mass spectrometer （HPLC-MS/MS）. After removed oil of the sample by N-hexane, extracted by 0.2% Formic acid-0.05mo]/L Ammonium Acetate buffer, centrifuged supernate and precipitated by acetonitrile after testing. The results show that the two kinds of compound has a well linear relationship among the range of 1.0 - 50.0 u g/L; Limits Of Quantification （ LOQ ）： ehlormequat was 0.32？g/L,mepiquat chloride was 0.45？g/L; the recovery rates were 91.7%~94.3%; relative standard deviation were 3.9%-6.1%; The measured results show that 30% of the sample contained 11.2？g/kg to 78.47g/kg were chlormequat, and 9.7？g/kg to 126.67g/kg were mepiquat chloride ; This method was simple,rapid, sensitive and precise, it could be used as a rapid detection and quantitative analysis method for pesticide residue of forage.