中国饲料
中國飼料
중국사료
CHINA FEED
2015年
13期
29-37
,共9页
类固醇激素%蛋类产品%液相色谱-串联质谱%主成分分析
類固醇激素%蛋類產品%液相色譜-串聯質譜%主成分分析
류고순격소%단류산품%액상색보-천련질보%주성분분석
steroids%eggs%liquid chromatography-tandem mass spectrometry%principal component analysis
本实验采用高效液相色谱-电喷雾质谱法对禽蛋类产品中的26种类固醇激素进行了测定。实验过程包括乙腈提取、ZnCl2去除磷脂、PLEXA固相萃取柱净化等。柱后注射法观察ZnCl2去除磷脂效果，并对固相萃取条件进行了优化。实验结果表明，应用酶水解法测定游离或结合态的类固醇激素精确性好（RSD≤15%），本方法的定量限为0.05~25 ng/g，平均回收率为63.2%~121.5%。该法可用于检测不同种类（鸡蛋、鸭蛋、鹌鹑蛋、鸽子蛋）与不同养殖方式（普通鸡蛋、有机鸡蛋）的蛋类产品，具有灵敏度高，实用性强等特点。此外，此法也可进行类固醇激素残留检测，为食品安全风险评估提供参考依据。
本實驗採用高效液相色譜-電噴霧質譜法對禽蛋類產品中的26種類固醇激素進行瞭測定。實驗過程包括乙腈提取、ZnCl2去除燐脂、PLEXA固相萃取柱淨化等。柱後註射法觀察ZnCl2去除燐脂效果，併對固相萃取條件進行瞭優化。實驗結果錶明，應用酶水解法測定遊離或結閤態的類固醇激素精確性好（RSD≤15%），本方法的定量限為0.05~25 ng/g，平均迴收率為63.2%~121.5%。該法可用于檢測不同種類（鷄蛋、鴨蛋、鵪鶉蛋、鴿子蛋）與不同養殖方式（普通鷄蛋、有機鷄蛋）的蛋類產品，具有靈敏度高，實用性彊等特點。此外，此法也可進行類固醇激素殘留檢測，為食品安全風險評估提供參攷依據。
본실험채용고효액상색보-전분무질보법대금단류산품중적26충류고순격소진행료측정。실험과정포괄을정제취、ZnCl2거제린지、PLEXA고상췌취주정화등。주후주사법관찰ZnCl2거제린지효과，병대고상췌취조건진행료우화。실험결과표명，응용매수해법측정유리혹결합태적류고순격소정학성호（RSD≤15%），본방법적정량한위0.05~25 ng/g，평균회수솔위63.2%~121.5%。해법가용우검측불동충류（계단、압단、암순단、합자단）여불동양식방식（보통계단、유궤계단）적단류산품，구유령민도고，실용성강등특점。차외，차법야가진행류고순격소잔류검측，위식품안전풍험평고제공삼고의거。
A means employed liquid chromatography with tandem mass spectrometry (LC-MS/MS) in electrospray ionization mode(ESI)for analyzing 26 steroids in egg was constructed.The step included extraction with acetonitrile and re-moval of phospholipids by zinc chloride(ZnCl2) before SPE cleanup with a Plexa cartridge.The effect of ZnCl2 on phospho-lipid removal was directly observed using the post column infusion and SPE washing and elution conditions were optimized using a shallow gradient procedure.The results indicated that enzyme hydrolysis was used to determine free and conjugated steroids and satisfactory precision (RSD≤15%) was aquired, the limits of quantification were between 0.05 and 25 ng/g depending on steroid types,the recoveries ranged from 63.2%to 121.5%and this method was effectively employed to com-pare the steroids in eggs belonging to different species (i.e., hen,duck,quail and pigeon eggs) or different raising system (i.e., normal vs.organic eggs).The developed method is sensitive and useful for detection and quantification of steroids in eggs and can be used for residue control programs.Furthermore,the acquired steroid content will provide a reference for food risk assessment analysis.
