采用液相色谱-串联质谱法测定动物肾脏脂肪中各种乙酰基孕甾酮的确证方法。
Confirmatory method for the determination of various acetylgestagens in animal kidney fat using liquid chromatography-tandem mass spectrometry.
机构信息
The State Laboratory, Backweston, Celbridge, Co., Kildare, Ireland.
出版信息
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2009 May;26(5):672-82. doi: 10.1080/02652030802642110.
A confirmatory method has been developed and validated that allows for the simultaneous detection of medroxyprogesterone acetate (MPA), megestrol acetate (MGA), melengestrol acetate (MLA), chlormadinone acetate (CMA) and delmadinone acetate (DMA) in animal kidney fat using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The compounds were extracted from kidney fat using acetonitrile, defatted using a hexane wash and subsequent saponification. Extracts were then purified on Isolute CN solid-phase extraction cartridges and analysed by LC-MS/MS. The method was validated in animal kidney fat in accordance with the criteria defined in Commission Decision 2002/657/EC. The decision limit (CCalpha) was calculated to be 0.12, 0.48, 0.40, 0.63 and 0.54 microg kg(-1), respectively, for MPA, MGA, MLA, DMA and CMA, with respective detection capability (CCbeta) values of 0.20, 0.81, 0.68, 1.07 and 0.92 microg kg(-1). The measurement uncertainty of the method was estimated at 16, 16, 19, 27 and 26% for MPA, MGA, MLA, DMA and CMA, respectively. Fortifying kidney fat samples (n = 18) in three separate assays showed the accuracy of the method to be between 98 and 100%. The precision of the method, expressed as % RSD, for within-laboratory reproducibility at three levels of fortification (1, 1.5 and 2 microg kg(-1) for MPA, 5, 7.5 and 10 microg kg(-1) for MGA, MLA, DMA and CMA) was less than 5% for all analytes.
已经开发并验证了一种确证方法，该方法允许使用液相色谱-串联质谱法（LC-MS/MS）同时检测动物肾脂肪中的醋酸甲地孕酮（MPA）、醋酸美仑孕酮（MGA）、醋酸美雄酮（MLA）、醋酸氯地孕酮（CMA）和醋酸去甲孕酮（DMA）。用乙腈从肾脂肪中提取化合物，用己烷洗涤脱脂，然后进行皂化。然后将提取物用 Isolute CN 固相萃取小柱纯化，并通过 LC-MS/MS 进行分析。该方法按照委员会决定 2002/657/EC 定义的标准在动物肾脂肪中进行了验证。决策限（CCalpha）分别计算为 0.12、0.48、0.40、0.63 和 0.54μgkg-1，用于 MPA、MGA、MLA、DMA 和 CMA，相应的检测能力（CCbeta）值分别为 0.20、0.81、0.68、1.07 和 0.92μgkg-1。该方法的测量不确定度估计分别为 MPA、MGA、MLA、DMA 和 CMA 的 16%、16%、19%、27%和 26%。在三个独立的测定中，对肾脂肪样品（n=18）进行加标，表明该方法的准确度在 98%至 100%之间。该方法的精密度，用 %RSD 表示，在三个加标水平（MPA 的 1、1.5 和 2μgkg-1，MGA、MLA、DMA 和 CMA 的 5、7.5 和 10μgkg-1）的实验室重复性内，所有分析物的精密度均小于 5%。
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