摘要
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。
The effective method of liquld-liquid extraction ( LLE ) -solid phase extraction ( SPE ) -high performance liquid phase chromatography ( HPLC ) was developed to determine 5kinds of sexy hormones in milk powder and chicken. The unit- ed technology of LLE and SPE was used for purification treat- ment and the kinds of extraction solution and SPE column was optimized. Meanwhile qualitative and quantitative analysis was applied with reversed-phase C18 and gradient elution mode of HPLC. The results indicated that the excellent linearity rela- tion of target analytes was in wide concentration' ranges of 1.0 ~ 200. 0 μg/mL and the limit of detection was 4. 7 - 21.0 μg/kg. The recoveries were 88.8% - 104. 2% and rel- ative standard deviation (RSD) was less than 7.2%. 5 sexy hormones were not detected in 10 batches of milk powder and chicken samples provide by municipal quality supervision. This method is sensitive, reliable and shows good application prospect in enrichment and separation of practical food sam- ples.
出处
《化学试剂》
CAS
CSCD
北大核心
2013年第6期522-526,共5页
Chemical Reagents
关键词
性激素
液液萃取-固相萃取
高效液相色谱
乳粉
鸡肉
sexy hormones
liquid-liquid extraction-solid phase extraction
HPLC
milk powder
chicken