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A simple toxicological analysis of anabolic steroid preparations from the black market

机译:来自黑市的合成代谢类固醇制剂的简单毒理分析

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Objectives: A simple and rapid gas chromatography (GC) method with mass spectrometry (MS) detection was developed for the identification and quantification of anabolic steroids in pharmaceutical preparations from the black market. Material and Methods: After a liquid-liquid extraction of pharmaceutical products at acidic, neutral and basic pH with chloroform-isopropanol (9:1, v/v), the different steroids were separated by fused silica capillary column and detected by electron impact (EI)-MS in positive ionization mode. Results and Conclusion: The assay was validated in the range from 10 mg to 250 mg/g powder preparations and 0.02 mg to 200 mg/mL liquid preparations with good determination coefficients (r~2 ≥ 0.99) for the calibration curves. At three concentrations spanning the linear dynamic ranges of the calibration curves, mean recoveries were always higher than 90% and intra-assay and inter-assay precision and accuracy were always better than 15%. This method was successfully applied to the analysis of 15 pharmaceutical preparations sold by illegal sources. In only two cases the content was the one reported on the labels. In the other cases, no substances at all, or steroids different from those reported on the labels or different amounts from those declared were found.
机译:目的:建立了一种简单快速的气相色谱(GC)方法和质谱(MS)检测方法,用于鉴定和定量黑市药品中的合成代谢类固醇。材料和方法:用氯仿-异丙醇(9:1,v / v)在酸性,中性和碱性pH值下进行液-液萃取药物产品后,通过熔融硅胶毛细管柱分离不同的类固醇,并通过电子碰撞检测( EI)-MS处于正电离模式。结果与结论:该方法在10 mg至250 mg / g粉末制剂和0.02 mg至200 mg / mL液体制剂中得到验证,校正曲线的测定系数很好(r〜2≥0.99)。在跨越校准曲线线性动态范围的三个浓度下,平均回收率始终高于90%,而批内和批间精密度和准确性始终高于15%。该方法已成功地用于分析非法来源销售的15种药物制剂。只有两种情况是标签上报告的内容。在其他情况下,根本没有发现与标签上报告的物质不同或与声明的物质含量不同的类固醇。

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