%0 Journal Article %T Quick determination of 39 hormones residues in infant formula by liquid chromatography-tandem mass spectrometry
液相色谱-串联质谱法快速测定婴幼儿配方奶粉中39种激素残留量 %A ZHU Weixia %A LIU Yafeng %A YUAN Ping %A YANG Jizhou %A
祝伟霞 %A 刘亚风 %A 袁萍 %A 杨冀州 %J 色谱 %D 2010 %I %X A quick confirmative method was developed for determining the residues of 17 glucocorticoids, 11 progesterones, 3 androgens and 8 estrogens in infant formula by liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS). The sample was extracted with acetonitrile at first. Then the lipid substances were removed by centrifugation under freezing condition and liquid-liquid extraction with hexane of the extract. The purification was carried out on hydrophilic-lipophilic solid-phase extraction columns and methanol was used as the eluted solvent. The detection of 39 analytes was carried out in the positive or negative multi-reaction monitoring (MRM) mode, separately. Acetonitrile-0.1% formic acid was used as the mobile phase and an ordinary silica gel C18 column was selected to separate the analytes in the positive mode. Acetonitrile-0.1% aqueous ammonia as mobile phase and the separation was carried out on an ultra-performance C18 column with a wide pH range in the negative mode. The limits of quantification (LOQ, S/N≥10) were 0.02~5 μg/kg. The overall recoveries varied from 59.5% to 117.9%, and the relative standard deviations (RSD) were between 6.4% and 16.3%. The real sample tests showed that the simple and accurate method can be used for determining the residues of multi-endogenous and chemically synthesized hormones in milk powders. %K liquid chromatography-tandem mass spectrometry (LC-MS/MS) %K solid-phase extraction (SPE) %K frozen delipidation %K hormones %K infant formula
液相色谱-串联质谱 %K 固相萃取 %K 冷冻除脂 %K 激素 %K 婴幼儿奶粉 %U http://www.alljournals.cn/get_abstract_url.aspx?pcid=6E709DC38FA1D09A4B578DD0906875B5B44D4D294832BB8E&cid=6579068328FE643F&jid=4D81E042D77AFEC6881D14759692069C&aid=D610C80DE192A0D5E7BA3550B4DB2C64&yid=140ECF96957D60B2&vid=D3E34374A0D77D7F&iid=708DD6B15D2464E8&sid=D7513DBF373F2B6C&eid=1F51A4E3D1D75885&journal_id=1000-8713&journal_name=色谱&referenced_num=0&reference_num=12