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首页> 外文期刊>Analytica chimica acta >Rapid method for the determination of stanozolol in meat with supercritical fluid extraction and liquid chromatography-mass spectrometry
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Rapid method for the determination of stanozolol in meat with supercritical fluid extraction and liquid chromatography-mass spectrometry

机译：超临界流体萃取-液相色谱-质谱法快速测定肉中西坦唑

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摘要

Stanzolol is isolated from animal tissues, such as bovine meat by automated supercritical fluid extraction (SEE). After the additiom of the internal standard stanoolol-d3 and sample pretreatment, the analytes are extracted from the matrix by supercritical CO_2 and trapped directly in-line on aminopropyl placed in the extraction vessel. The samples are analysed by liquid chromatography combined with single quad mass selective detection liquid chromatography-mass spectrometry (LC-MS) for screening and quantification and ion-trap mass selective detection (LC-MS~n) for confirmation of the identity. For quantification, the deuterated internal standard is added and the protonated molecule of the analyte and internal standard are monitored. For configuration of the identity of the analyte, two transition ions (two MS/MS ions) are monitored and the ratios between the ions are calculated and compared with those of standards. The detection limit of the screening method is 0.2 mug kg~(-1), the limit of identification is 0.5 mug kg~(-1).The mean within-laboratory reproducibility ranges from 11-18% (%R.S.D.) at the concentration level of 0.5-5 mug kg~(-1) (n = 18).Running the SFE procedure overnight allows the analysis of 24 samples of meat per day.
机译：通过自动超临界流体萃取（SEE）从动物组织（例如牛肉）中分离出斯坦唑醇。加入内标stanoolol-d3并进行样品预处理后，通过超临界CO_2从基质中提取分析物，并将其直接在线捕获在放置在提取容器中的氨丙基上。样品通过液相色谱与单四极杆质量选择检测液相色谱-质谱（LC-MS）结合进行分析和定量，并通过离子阱质量选择性检测（LC-MS_n）进行身份分析。为了进行定量，添加了氘化内标，并监测了分析物和内标的质子化分子。为了配置分析物的身份，需要监测两个过渡离子（两个MS / MS离子），并计算离子之间的比例并将其与标准样品进行比较。筛选方法的检出限为0.2杯kg〜（-1），鉴定的限度为0.5杯kg〜（-1）。浓度范围内的实验室平均再现性为11-18％（％RSD）水平为0.5-5杯子kg〜（-1）（n = 18）。整夜运行SFE程序可以每天分析24个肉样品。

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