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液相色谱-高分辨质谱法分析食品中的勃起功能障碍药物及其类似物。

Liquid chromatography-high-resolution mass spectrometry analysis of erectile dysfunction drugs and their analogues in food products.

机构信息

Centre for Forensic Science, University of Technology Sydney, Ultimo, NSW 2007, Australia; Pharmacy Enforcement Division, Ministry of Health, Petaling Jaya, Selangor 46200, Malaysia.

Centre for Forensic Science, University of Technology Sydney, Ultimo, NSW 2007, Australia.

出版信息

Forensic Sci Int. 2021 May;322:110748. doi: 10.1016/j.forsciint.2021.110748. Epub 2021 Mar 4.

Abstract

The presence of erectile dysfunction (ED) drugs in adulterated dietary supplements, mainly in pharmaceutical dosage forms, is frequently addressed in the literature. Little attention is given to food products despite their increasing adulteration trend. To address this knowledge gap targeted, suspected-target, and non-targeted strategies were utilised to analyse ED drugs and their analogues in powdered drink mix (PDM), honey, jelly, hard candy, and sugar-coated chewing gum using liquid chromatography-high-resolution mass spectrometry (LC-HRMS). The method was optimised and validated using 23 target analytes, representing different ED drugs with structural similarities. The modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction exhibited insignificant matrix effect (ME) within - 9.2-8.8% and provided complete coverage of target analytes with acceptable extraction recovery (RE) within 75.5-123.9%, except for carbodenafil in the PDM matrix. Based on the ME and RE performance, the analytical method was validated to analyse 25 food samples that claimed to enhance male sexual performance. The method exhibited good specificity and linearity with a limit of detection within 10-70 ng/mL and limit of quantification of 80 ng/mL. Similarly, the accuracy and precision were satisfactory within 77.4-122.0% and< 16.7%RSD, respectively. The LC-HRMS targeted analysis, together with suspected-target and non-targeted screenings, identified and detected ten ED drugs from 24 food samples. The modified QuEChERS extraction with LC-HRMS-based method was demonstrated to be universally applicable to various food products, covering an extensive range of known and potentially novel ED drugs, which is valuable for routine casework.

摘要

掺伪膳食补充剂(主要为药物剂型)中存在勃起功能障碍(ED)药物的情况在文献中经常被提及。尽管食品掺伪的趋势日益增加,但却很少受到关注。为了弥补这一知识空白,我们采用了有针对性的、疑似目标和非靶向策略,利用液相色谱-高分辨质谱(LC-HRMS)对粉末饮料混合物(PDM)、蜂蜜、果冻、硬糖和糖衣口香糖中的 ED 药物及其类似物进行分析。该方法使用 23 种具有结构相似性的不同 ED 药物的目标分析物进行了优化和验证。经改良的快速、简便、廉价、有效、耐用、安全(QuEChERS)提取法的基质效应(ME)在-9.2%至 8.8%之间,对目标分析物的覆盖率完全,除 PDM 基质中的卡泊非拉外,其提取回收率(RE)在 75.5%至 123.9%之间,可接受。基于 ME 和 RE 的性能,该分析方法对声称能增强男性性功能的 25 种食品样品进行了验证。该方法具有良好的特异性和线性,检出限为 10-70ng/mL,定量限为 80ng/mL。同样,准确度和精密度也令人满意,分别为 77.4%至 122.0%和<16.7%RSD。LC-HRMS 靶向分析与疑似目标和非靶向筛查相结合,从 24 种食品样品中鉴定和检测出 10 种 ED 药物。改良的 QuEChERS 提取法与基于 LC-HRMS 的方法相结合,证明对各种食品具有普遍适用性,涵盖了广泛的已知和潜在新型 ED 药物,这对常规案例工作非常有价值。

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