Simultaneous Determination of 8 Steroid Hormones in Feed by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry
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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,5 μm)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0~10 μg/L范围内线性相关系数(r)≥0.9995;检出限为0.10~0.34 μg/kg(S/N≥3),定量限为0.35~0.98 μg/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。
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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
Abstract: 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. -
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