单 位：
上海出入境检验检疫局动植物与食品检验检疫技术中心;上海大学生命科学学院
关键词：
超高效液相色谱-三重四极杆质谱;雄激素;孕激素;饲料
摘 要：
建立了同时测定饲料中勃地酮、甲睾酮、诺龙、群勃龙、甲羟孕酮乙酸酯、美仑孕酮、乙酸甲地孕酮和17α-羟基孕酮8种类固醇激素的超高效液相色谱-三重四极杆质谱(UPLC-MS/MS)检测方法。考察了提取溶剂,除蛋白和除脂条件对8种类固醇激素回收率的影响,最终选择乙腈为提取溶剂,用三氯乙酸和氢氧化钠除蛋白,用氯化镁和正己烷除脂,样品经Athena C18-WP(2.1×150 mm,5μm)色谱柱分离,以5 mmol/L乙酸铵(1‰甲酸)和乙腈(1‰甲酸)进行梯度洗脱,正离子电喷雾电离多反应监测模式测定,内标法进行定量分析。结果显示,8种化合物在0～10μg/L范围内线性相关系数(r)≥0.9995;检出限为0.10～0.34μg/kg(S/N≥3),定量限为0.35～0.98μg/kg(S/N≥10)。方法的平均回收率范围为70.4%～109%,相对标准偏差为0.38%～10.3%(n=6)。该方法操作简单,灵敏度高,重复性好,适用于饲料中8种类固醇激素的快速检测。
译 名：
Simultaneous Determination of 8 Steroid Hormones in Feed by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry
作 者：
FANG Ke-yan;ZHAO Chao-min;CHEN Qin;DENG Xiao-jun;School of Life Sciences,Shanghai University;Inspection and Quarantine Technology Center for Animal,Plant and Food,Shanghai Entry-Exit Inspection and Quarantine Bureau;
单 位：
FANG Ke-yan%ZHAO Chao-min%CHEN Qin%DENG Xiao-jun%School of Life Sciences,Shanghai University%Inspection and Quarantine Technology Center for Animal,Plant and Food,Shanghai Entry-Exit Inspection and Quarantine Bureau
关键词：
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS);;androgen;;progesterone;;feed
摘 要：
A method was developed for the screening and quantification of 8 steroid hormones including(boldenone,17-alpha-Methyltestosterone,19-Nortestosterone,trenbolone,medroxyprogesterone,melengestrol,megestrol-17-acetate,17-alpha-Hydroxyprogesterone)in feed by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The effects of extraction solvent,protein removal and degreasing conditions on the recovery of 8 steroid hormones were investigated. Finally,acetonitrile was selected as the extraction solvent,protein was removed with trichloroacetic acid and sodium hydroxide,and fat was removed with magnesium chloride and n-hexane. In the chromatographic analysis,the 8 target compounds were separated by Athena C18-WP(2.1×150 mm,5 μm)column and gradient elution with 5 mmol/L ammonium acetate(1‰ formic acid)and acetonitrile(1‰ formic acid),detected in positive multiple reaction monitoring(MRM)and quantified with internal standards. The results showed that the 8 steroid hormones exhibited good linear relationships in the range of 0～10 μg/L with correlation coefficients(r)of more than 0.9995;the limits of detection(LODs,S/N≥3)were 0.10～0.34 μg/kg and the limits of quantification(LOQs,S/N≥10)were 0.35～0.98 μg/kg. Average recoveries were 70.4%～109% with relative standard deviation of 0.38%～10.3%(n=6). The method was simple,rapid,sensitive and reproducible,and was suitable for rapid screening and detection of 8 steroid hormones in feed.
