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机构地区:[1]北京化工大学化学工程学院,北京100029 [2]中国计量科学研究院化学计量与分析科学研究所,北京100013
出 处:《化学分析计量》2011年第3期26-29,共4页Chemical Analysis And Meterage
基 金:科技部国家科技支撑项目(2009BAK61B02);科技部创新方法专项(2008IM021900);质检总局食品安全专项(21-ASPAQ1101);质检总局食品安全专项(ASPAQ0809-1009)
摘 要:建立了高效液相色谱法同时测定牛肉组织中勃地龙、诺龙、美雄酮、甲基睾酮、丙酸睾酮和丙酸诺龙的分析方法。试样经乙腈提取,冷冻离心脱脂净化,以甲醇-水为流动相,梯度洗脱,流速为1.0mL/min。该方法的检出限(LOD)为0.0051~0.0086mg/kg,定量限(LOQ)为0.0220~0.0287mg/kg,在0.25~10mg/L的线性范围内,相关系数一均大于0.999。在0.4mg/kg和2.0mg/kg的添加水平上,上述6种激素的平均回收率为84.1%~100.0%,测定结果的相对标准偏差为0.5%-3.5%(n=5)。该方法的样品前处理简单、快速、稳定性好,可用于牛肉组织中上述6种蛋白同化类激素的同时测定。A HPLC method was established for the simultaneous determination of six anabolic - androgenic steroids including methandienone, nandrolone, boldenone, methyltestosterone, testosterone propionate and nantrolone propionate in beef muscle tissues. The samples were extracted with acetonitrile and then cleaned up by freezing - lipid filtration. The mobile phase consisted of methanol - water at flow rate of 1.0 mL/min. The detection limits for the method were 0. 0051 -0.008 6 mg/kg, and the limits of quantification were 0. 0220 -0.028 7 mg/kg. The linear calibration curves were obtained in the concentration range of 0.25 - 10 mg/L, with r2 more than 0. 999. The recoveries of the six compounds were 84.1% - 100.0% fortified at the 0.4 mg/kg and 2.0 mg/kg levels, and the relative standard deviations of determination results were 0.5% - 3.5% ( n = 5 ). The established method is simple, rapid, sensitive and specific, and it is appropriate for the identification and quantification of anabolic androgenic steroids in animal muscle tissues.
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