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3'-羟基苯丙酸诺龙的气相色谱/高分辨质谱确证的样品净化程序。

Sample purification procedure for confirmation of 3'-hydroxy stanozolol by gas chromatography/high resolution mass spectrometry.

机构信息

Dope Control Center, Sports Authority of India, J. N. Stadium, New Delhi, India.

出版信息

Indian J Pharmacol. 2008 Aug;40(4):164-9. doi: 10.4103/0253-7613.43163.

Abstract

OBJECTIVE

To improve the detection limit of 3'-hydroxy-stanozolol by using the double extraction procedure, specific for basic drugs.

MATERIALS AND METHODS

The urine samples were spiked in four replicates with 3'-hydroxy-stanozolol at different concentrations of 1, 2, 5 and 10 ng/mL, processed by two different methods and injected into gas chromatography/high resolution mass spectrometry (GC-HRMS) instrument. The data was analyzed by comparing the recovery values and the ion match criterion of the two procedures.

RESULTS

The results show that the recovery percentage and ion match criterion of 3'-hydroxy-stanozolol at lower concentrations has a significant improvement when Solid phase extraction was performed, instead of Liquid-liquid extraction in the second extraction procedure.

CONCLUSION

The sample preparation procedure using Oasis-MCX cartridges allows confirmation of 3'-hydroxy-stanozolol at the minimum required performance limit (MRPL) decided by the World Anti Doping Agency. This procedure may be used for the confirmation of suspicious samples found in routine testing, as it efficiently fulfills the ion-matching criterion laid down by the World Anti Doping Agency.

摘要

目的

通过使用针对碱性药物的双重提取程序,提高 3'-羟基雄甾酮的检测限。

材料与方法

将尿样以 1、2、5 和 10ng/mL 的四个不同浓度在四个重复中加入 3'-羟基雄甾酮,用两种不同的方法进行处理,然后注入气相色谱/高分辨率质谱(GC-HRMS)仪器。通过比较两种程序的回收值和离子匹配标准来分析数据。

结果

结果表明,在第二提取程序中使用固相萃取代替液液萃取时,较低浓度下 3'-羟基雄甾酮的回收率和离子匹配标准有显著提高。

结论

使用 Oasis-MCX 小柱的样品制备程序可以确认世界反兴奋剂机构规定的最低性能限度(MRPL)的 3'-羟基雄甾酮。该程序可用于确认常规检测中发现的可疑样本,因为它有效地满足了世界反兴奋剂机构规定的离子匹配标准。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/b13a/2792608/21673dba522d/IJPharm-40-164-g001.jpg

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