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应用 LC-MS/MS 和 UHPLC-Q-Orbitrap 方法测定非法膳食补充剂和其他样品类型中的 54 种甾体

Application of LC-MS/MS and UHPLC-Q-Orbitrap methods for determining 54 steroids in illegal dietary supplements and other sample types.

机构信息

National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Center for Advanced Analysis, Cheongju, Republic of Korea.

出版信息

Rapid Commun Mass Spectrom. 2022 Aug 30;36(16):e9334. doi: 10.1002/rcm.9334.

DOI:10.1002/rcm.9334
PMID:35705484
Abstract

RATIONALE

With the development of the Internet and social network services, the public access to or use of illegal products has been increased via on/offline black markets. Steroids refer to the compounds yielding strong treatment effects on some diseases or muscle building, and are classified as the pharmaceutical compounds that are prohibited for personal use without a prescription. The prohibition is made for their potential risk to cause serious adverse effects along with their efficacies.

METHODS

To monitor the distribution of illicit products containing steroids, a simple and reliable analytical method was established and validated, allowing rapid and simultaneous determination of 54 steroids in them. During the screening, LC-Q-Orbitrap/MS was performed first followed by quantitative analysis using LC-MS/MS. For the accurate and reliable analysis, the samples were extracted using QuEChERS to reduce the matrix effect.

RESULTS

After the screening of 617 illegal samples advertised as being effective in alleviating various diseases or improving athletic performance with the established LC-Q-Orbitrap/MS method, the validated LC-MS/MS method was used to perform the quantitative analysis of the detected steroids. Of these, 142 samples were adulterated with steroids, and several samples with two or more steroids were detected. Due to the lack of previous studies on the toxicity of these illicit products, the side effects of consuming them are unpredictable and could be harmful.

CONCLUSIONS

The development of LC-Q-Orbitrap/MS method accompanied by LC-MS/MS could be successfully applied to the inspection of illegal steroid products for public health, enabling the rapid and accurate detection of analytes and incorporation of non-analyte components.

摘要

理由

随着互联网和社交网络服务的发展,公众通过线上和线下黑市获得或使用非法产品的机会增加了。类固醇是指对某些疾病或肌肉生长具有强大治疗效果的化合物,被归类为未经处方禁止个人使用的药物化合物。之所以禁止使用,是因为它们可能具有严重不良反应的风险,同时也具有疗效。

方法

为了监测含有类固醇的非法产品的分布,建立并验证了一种简单可靠的分析方法,允许快速同时测定其中的 54 种类固醇。在筛选过程中,首先进行 LC-Q-Orbitrap/MS 分析,然后使用 LC-MS/MS 进行定量分析。为了进行准确可靠的分析,使用 QuEChERS 提取样品以减少基质效应。

结果

使用建立的 LC-Q-Orbitrap/MS 方法对 617 种声称可有效缓解各种疾病或提高运动表现的非法样本进行筛选后,使用经过验证的 LC-MS/MS 方法对检测到的类固醇进行定量分析。其中,142 种样品中掺有类固醇,并且检测到几种含有两种或更多种类固醇的样品。由于这些非法产品的毒性以前没有研究过,因此食用它们的副作用是不可预测的,可能会有害。

结论

LC-Q-Orbitrap/MS 方法与 LC-MS/MS 一起开发可成功应用于公共健康领域的非法类固醇产品检验,能够快速准确地检测分析物并包含非分析物成分。

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