【摘要】 目的建立固相微萃取-高效液相色谱法(SPME-HPLC)同时测定牛奶和肉类食品中己烯雌酚、丙酸睾酮和双酚A的方法。方法牛奶和肉类样品经80%甲醇溶液超声提取后,加乙腈和正己烷沉淀蛋白并除脂,用固相微萃取进行萃取和浓缩,由C18液相色谱柱分离测定。采用85μm PA作为萃取头,样品提取液在(60±2)℃下萃取40 min,乙腈中静态脱附5 min后进行高效液相色谱分析,内标法定量。结果 3种化合物的线性范围为0.001μg/ml~5.0μg/ml,相关系数(r)为0.992~0.999,检出限为0.001μg/ml~0.01μg/ml,回收率为92.2%~115%,相对标准偏差为1.2%~14.3%。此法用于测定肉类和牛奶样品,牛肉、精腿猪肉、牛奶样品中检出己烯雌酚,牛肉和鸡皮中检出丙酸睾酮,所检样品中未检出双酚A。结论本法前处理采用固相微萃取,操作简单、准确、环保,可用于牛奶和肉类样品中己烯雌酚、丙酸睾酮和双酚A测定。更多还原

【Abstract】 Objective A method was developed for the simultaneous determination of diethylstilbestrol( DES),testosterone propionate( TES) and bisphenol A( BPA) in milk and meat based on solid phase micro-extraction( SPME) and high-performance liquid chromatography( HPLC).Methods The samples were extracted with 80% methanol with the assistance of ultrasonic,and proteins and lipids in the extracted solution were precipitated and removed with acetonitrile and hexane.The extraction and condense were carried out by solid phase micro-extraction,and 3 compounds were separated and analyzed using C18 column.The extractions were carried out in 85 μm PA( polyacrylate) fiber and the best results were found with 40 minutes of extraction at( 60 ± 2) °C,and then 5 minutes of desorption in acetonitrile for HPLC determination.The results were calculated by internal standard method.Results The linear ranges were 0.001 μg/ml-5.0 μg/ml.The correlation coefficients( r) were within 0.992-0.999,and the detection limits of 3 kinds of compounds were within 0.001 μg/ml-0.01 μg/ml.The recoveries were within 92.2%-115%,and the RSD was within 1.2%-14.3%.The optimized method has been applied to determine the target compounds in milk and meat samples.The analysis revealed the presence of diethylstilbestrol in beef,fine leg of pork and milk,testosterone propionate in beef and chicken skin and no bisphenol A in the samples.Conclusion The described method showed a good performance,which is simple,accurate,and green.It can be used to determine diethylstilbestrol,testosterone propionate and bisphenol A in milk and meat samples.更多还原