高效液相色谱法测定猪组织中残留的咪唑苯脲

摘要

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 j8-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.%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1 mol/L盐酸提取,再用正已烷-异戊醇(3∶2,v/v)混合溶剂萃取净化.以乙腈和0.0075 mol/L戊烷磺酸钠水溶液(含0.1％三乙胺,pH 3.0)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～ 10000 μg/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10 μg/kg,定量限(LOQ)为20 μg/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.