【摘要】 目的优化动物性食品中盐酸克仑特罗残留的高效液相色谱法(HPLC)检测条件,建立可大批量测定样品的方法。方法样品经高氯酸溶液超声提取,乙酸乙酯-异丙醇萃取,有机相浓缩后,采用Agilent C18(150 mm×4.6 mm,5μm)色谱柱进行分离,流动相为甲醇-磷酸二氢钠溶液,采用高效液相色谱仪进行分析。结果标准物质在0.2~10.0μg/m L时,方法的线性关系良好,相关系数(r)=0.999 84;方法的检测限为0.15μg/kg,低于国标方法的0.5μg/kg。盐酸克仑特罗保留时间为6.51 min,峰形良好;加标质量为1.6~12μg时,加标回收率为92.86%~100.93%,高于国标方法 (89.79%~92.36%);日内精密度和日间精密度均小于5%,低于国标方法。结论优化后的色谱条件适用于动物性食品中盐酸克仑特罗的大批量测定。更多还原

【Abstract】 Objective To establish a high performance liquid chromatography(HPLC) through the optimization of the chromatographic conditions,which can detect the contents of clenbuterol hydrochloride(CL) residues in animal edible product in a large quantity. Methods The animal edible product were extracted by perchloric acid,and then impurities were removed by liquid-liquid extraction(LLE) which used ethyl acetate-isopropanol. After the organic phase was concentrated, C18 column(150 mm×4.6 mm,5 μm) was used to separate CL. Mobile phase were methanol-sodium dihydrogen phosphate,and then determined by HPLC. Results A good linear response was obtained over the range of 0.2-10.0 μg/m L with the correlation coefficient(r) 0.999 84. The method determination limit was 0.15 μg/kg which was lower than the National standard method 0.5μg/kg. The retention time of the CL was 6.51 min,the chromatographic peak was good. The recovery rates spiked with standards1.6-12 μg were 92.86%-100.93%, which was higher than National standard method(89.79%-92.36%). The precision of intra-day and inter-day were both under 5%,which lower than National standard. Conclusion The optimized chromatographic conditions are suitable for the large quantity determination of clenbuterol hydrochloride in animal edible product.更多还原