高效液相色谱法测定猪组织中残留的咪唑苯脲

Determination of imidocarb residue in swine tissues by high performance liquid chromatography

建立了高效液相色谱(HPLC)测定猪可食性组织中咪唑苯脲残留的方法。猪组织经β-葡萄糖苷酶水解后,用1mol/L盐酸提取,再用正己烷-异戊醇(3∶2,v/v)混合溶剂萃取净化。以乙腈和0.0075mol/L戊烷磺酸钠水溶液(含0.1%三乙胺,pH3.0)作为流动相,经C18反相色谱柱分离后用紫外检测器检测。结果表明:该方法在咪唑苯脲含量为10～10000μg/L范围内呈现良好的线性关系,相关系数大于0.999;空白组织中加标样品的检出限(LOD)为10μg/kg,定量限(LOQ)为20μg/kg。在定量限、最高残留限量(MRL)、2倍MRL添加水平下,不同组织的平均回收率为80.04%～110.32%,相对标准偏差为0.82%～10.00%。表明该检测方法简单、灵敏,适用于猪组织中咪唑苯脲残留的定量检测。

A quantitive method for the determination of imidocarb residue in edible tissues of swine by high performance liquid chromatography（HPLC） was developed.The analyte was digested by β-glucosidase first,and then extracted with 1 mol/L hydrochloric acid.The aqueous phase was back-extracted with the mixture of hexane-isoamyl alcohol（3∶2,v/v） for the purification.The mobile phases were acetonitrile（phase A） and 0.007 5 mol/L 1-pentansulfonic acid sodium aqueous solution containing 0.1% triethylamine,adjusted to pH 3.0 with glacial acetic acid（phase B）.The analyte was detected by ultraviolet absorption spectroscopy after the separation was achieved on a C18 RP column.The linear range was 10-10 000 μg/L,and the correlation coefficient was more than 0.999.The limit of detection（LOD） was 10 μg/kg,and the limit of qualification（LOQ） was 20 μg/kg.The mean recoveries of imidocarb in swine tissues at the added levels of LOQ,MRL（maximum residue limit） and 2MRL ranged from 80.04% to 110.32%,and the relative standard deviations（RSDs） of intra-and inter-day analyses ranged from 0.82% to 10.00%.The method is simple and sensitive for the quantification of imidocarb residue in swine tissues.