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建立液液萃取(LLE)-固相萃取(SPE)-高效液相色谱(HPLC/DAD)方法对乳粉和鸡肉中5种性激素进行测定。实验采用LLE和SPE联合技术对复杂基质样品进行净化处理,优化了萃取过程中溶剂及固相萃取小柱种类。同时,采用反相C18色谱柱,梯度洗脱方式进行色谱定性、定量分析。结果表明,目标分析物在1.0～200.0μg/mL范围内有良好的线性相关性,方法检出限4.7～21.0μg/kg,方法回收率88.8%～104.2%,相对标准偏差<7.2%。应用该方法对市质检所送检的10批次乳粉和鸡肉样品进行分析,5种性激素均未检出。该方法灵敏、可靠,显示出其富集与分离实际食品样品中多种性激素的良好应用前景。
A total of 5 sex hormones in milk powder and chicken meat were determined by liquid-liquid extraction (LLE) -phase extraction-liquid chromatography-high performance liquid chromatography (HPLC / DAD) Experiments using LLE and SPE combined with complex matrix samples were purified to optimize the extraction process of solvent and SPE cartridges. At the same time, reversed-phase C18 column and gradient elution method were used for qualitative and quantitative analysis. The results showed that there was a good linear correlation between the target analytes and 1.0 ~ 200.0μg / mL. The detection limit was 4.7 ~ 21.0μg / kg, the recoveries were 88.8% -104.2% and the relative standard deviations were less than 7.2%. Application of the method of quality inspection of the city sent 10 batches of milk powder and chicken samples were analyzed, five kinds of sex hormones were not detected. The method is sensitive and reliable and shows its good application prospects for enrichment and separation of various sex hormones in real food samples.