饲料中玉米赤霉醇、玉米赤霉酮和己烯雌酚的测定——超高效液相色谱-串联质谱法  

Determination of Zearalanol, Zearalanone and Diethylstilbestrol in Feeds by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张天姝 马雷 玄兵 孙世峰 

机构地区：[1]辽宁省兽药饲料畜产品质量安全检测中心,辽宁沈阳110016 [2]辽宁省沈阳市兽药饲料监察所,辽宁沈阳110016 [3]辽宁省锦州市兽药饲料监察所,辽宁锦州110016 [4]辽宁省沈阳市动物卫生监督所,辽宁沈阳110000

出　　处：《现代畜牧兽医》2018年第2期18-23,共6页Modern Journal of Animal Husbandry and Veterinary Medicine

摘　　要：本文建立了饲料中玉米赤霉醇、玉米赤霉酮和己烯雌酚的UPLC-MS/MS分析方法。饲料样品经正己烷-乙酸乙酯溶液(V/V=85:15)提取,离心后提取液氮气吹干,正己烷溶解后经-OH净化柱净化,用50%乙腈水溶液洗脱,UPLC-MS/MS分析。结果表明,3种目标化合物药物在10.0~50.0μg/kg浓度范围内线性关系良好,r≥0.99。以玉米、DDGS、配合饲料、精料补充料等为添加基质,其回收率在61.7%~99.4%之间,检出限为10μg/kg,定量限为20μg/kg。说明本方法灵敏度高,专属性好,操作简单,结果可靠,可满足饲料中玉米赤霉醇、玉米赤霉酮和己烯雌酚的分析检测。A method of Ultra Performance Liquid Chromatography-Tandem mass spectrometry（UPLC-MS/ MS） for determination of Zearalanol, Zearalanone and Diethylstilbestrol in feeds was developed. The samples were separately extracted with N-hexane-ethylacetate（V/V=85：15） mixed solution, then the supernatant was evaporated to dryness under the nitrogen steam after centrifugated, dissolved in n-hexane. Then cleaned up with multifunetion cartridges and wash with 50% acetonitrile solu- tion, finally assayed by UPLC-MS/MS. The results showed that the limits of detection were 10.0 μg/ kg for Zearalanol, Zearalanone and Diethylstilbestrol, and the average recoveryies were 61.7%~ 99.4%. The real sample tests showed this method can be used for the sensitive and accurate deter- mination of Zearalanol, Zearalanone and Diethylstilbestrol in feeds.

关 键 词：玉米赤霉醇 玉米赤霉酮 己烯雌酚 饲料 UPLC-MS/MS 

分 类 号：TS207.53[轻工技术与工程—食品科学]