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首页> 外文期刊>The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry >Determination of acetyl gestagenic steroids inkidney fat by automated supercritical fluid extraction and liquid chromatography ion-trap mass spectrometry
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Determination of acetyl gestagenic steroids inkidney fat by automated supercritical fluid extraction and liquid chromatography ion-trap mass spectrometry

机译：自动化超临界流体萃取-液相色谱-离子阱质谱法测定乙酰孕激素类固醇肾上腺脂肪

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摘要

Gestagenic steroids are isolated from animal tissues such as bovine kidney fat by automated supercritical fluid extraction (SFE).After the addition of internal standards and sample pretreatment,the analytes are extracted from the matrix by supercritical CO_2 and trapped directly in-line on alumina placed in the extraction vessel.The samples are analysed by liquid chromatography combined with ion-trap mass selective detection (LC-MS~n).For quantification,deuterated internal standards are added and single ions of the anlaytes and internal standards are monitored.For confirmationof the identity of the analytes,two transitionions (one MS~2 and one MS~3) were monitored and the ratios between the ions were calcualted andcompared with those of standards.The detection capability for the multi-analyte LC-MS~n analysis of megestrol acetate (MA) is 0.5 #mu#g kg~(-1).The mean within-laboratory reproducibility ranges from 16-19%(%RSD) at a concentration level of 0.5 #mu#g kg~(-1) (n=9).Running the SFE procedure overnight allows the analysis of 24 samples of fat per day.
机译：通过自动超临界流体萃取（SFE）从牛肾脂肪等动物组织中分离出基因发生类固醇。添加内标并进行样品预处理后，通过超临界CO_2从基质中萃取分析物，并将其直接在线捕获在氧化铝上通过液相色谱结合离子阱质量选择检测（LC-MS〜n）对样品进行分析。为定量起见，添加了氘化的内标并监测了被分析物和内标中的单个离子。分析物的身份，监测两个离子对（一个MS〜2和一个MS〜3），并计算离子之间的比率并将其与标准品进行比较。对多分析物LC-MS〜n分析的检测能力醋酸孕甾酮（MA）为0.5＃mu＃g kg〜（-1）。实验室内的平均重现度为16-19％（％RSD），浓度为0.5＃mu＃g kg〜（-1） （n = 9）。一整夜的SFE程序每天可分析24个脂肪样品。

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