高效液相色譜-串聯(lián)質(zhì)譜法測定牛奶和雞肉中4種激素本底值
發(fā)布時間:2018-03-30 09:45
本文選題:激素 切入點:雞肉 出處:《食品科學(xué)》2017年22期
【摘要】:建立牛奶和雞肉中4種激素(睪酮、甲基睪酮、孕酮、氫化可的松)本底值同時測定的高效液相色譜-串聯(lián)質(zhì)譜方法。樣品經(jīng)β-葡萄糖醛酸酶/芳香基硫酸酯酶水解,加入乙腈超聲提取,正己烷除脂肪。采用ZORBAX SB-C18色譜柱分離,以0.1%甲酸溶液和甲醇為流動相梯度洗脫,分別在電噴霧離子源正、負離子模式下以多反應(yīng)監(jiān)測模式分段掃描同時檢測,基質(zhì)匹配外標法定量。結(jié)果表明,4種激素在相應(yīng)的質(zhì)量濃度范圍內(nèi)線性良好,相關(guān)系數(shù)均大于0.991;在牛奶中的檢出限(RSN=3)和定量限(RSN=10)分別為0.02~0.10μg/kg和0.06~0.33μg/kg,在雞肉中的檢出限和定量限分別為0.03~0.12μg/kg和0.10~0.40μg/kg;在3個水平下的平均回收率為牛奶56.0%~132.8%,雞肉79.6%~122.0%;相對標準偏差為牛奶1.8%~17.3%,雞肉2.0%~18.1%。該方法簡單、快速、準確,適用于對牛奶和雞肉中4種激素進行快速篩查和本底值測定。
[Abstract]:The samples were hydrolyzed by 尾 -glucuronidase / aromatic sulfate enzyme and extracted with acetonitrile.ZORBAX SB-C18 column was used to separate the samples, and 0.1% formic acid solution and methanol were used as mobile phase gradient elution. The results were detected simultaneously by multi-reaction monitoring mode in the mode of electrospray ion source and negative ion mode, respectively. The matrix matched external standard method was used to quantify the samples.The results showed that the four hormones were linear in the corresponding range of mass concentration.The difference is 1. 8 and 17. 3 and the chicken is 2. 0 and 18. 1.The method is simple, rapid and accurate. It is suitable for rapid screening and background determination of four hormones in milk and chicken.
【作者單位】: 中國檢驗檢疫科學(xué)研究院食品安全研究所;內(nèi)蒙古滿洲里出入境檢驗檢疫局技術(shù)中心;
【基金】:“十三五”國家重點研發(fā)計劃重點專項(2016YFD0401103;2016YFF0203903)
【分類號】:O657.63;TS207.3
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本文編號:1685387
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