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首页> 外文期刊>Journal of mass spectrometry: JMS >A high throughput approach for determination of dermorphin in human urine using liquid chromatography-mass spectrometry for doping control purposes
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A high throughput approach for determination of dermorphin in human urine using liquid chromatography-mass spectrometry for doping control purposes

机译：利用液相色谱 - 质谱法测定人尿液中皮肤的高通量方法，用于掺杂控制目的

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摘要

Dermorphin is a peptide with analgesic actions similar to morphine, but with greater effect and less potential to cause tolerance. The use of dermorphin has been documented in race horses, and its use in humans has already been reported. Considering the potential advantages from the use of dermorphin over morphine, a method to monitor it, and its main metabolite dermorphin (1-4) in humans becomes necessary for doping control. Here, we present two orthogonal methods for this purpose: a high-throughput liquid chromatography coupled to high-resolution mass spectrometry (HRMS) as an initial testing procedure and liquid chromatography-tandem mass spectrometry (MS/MS) in the selected reaction monitoring (SRM) acquisition mode for a confirmation procedure. For urine samples, pretreatment through a mixed-mode weak cation-exchange solid-phase extraction emerged as an effective approach to extract peptides from the biological sample. For the HRMS analysis, a full-MS scan acquisition mode was selected to detect the exact masses of dermorphin and dermorphin (1-4) atm/z803.37226 and 457.20816, respectively. The SRM method used in the MS/MS confirmation protocol presented high specificity and sensitivity. The selected product ions for dermorphin were 602.2, 202.1 and 574.3 and for dermorphin (1-4) were 207.1, 223.1, and 235.1. Both methods were evaluated for specificity, repeatability, carryover, matrix effects, and recovery. No carryover and matrix effects were detected. The limit of detection for initial testing procedure and the limit of identification for confirmation procedure was 2.5 ng/ml. Also, specificity and robustness were acceptable for the application. Together, the developed methods proved to be efficient for the analysis of dermorphin and metabolite for human doping control purpose.
机译：皮肤是一种肽，其具有与吗啡类似的镇痛作用，但具有更大的效果和造成耐受性的潜力。在比赛中已经记录了Dermorphin，已经报道了对人类的使用。考虑到使用Dermorphin对吗啡的潜在优势，一种监测它的方法，以及人类的主要代谢性皮肤（1-4）对于掺杂控制是必要的。在这里，我们提出了两个正交方法：在所选反应监测中，偶联至高分辨率质谱（HRMS）作为初始测试程序和液相色谱 - 串联质谱（MS / MS）的高通量液相色谱。 SRM）确认程序的采集模式。对于尿液样品，通过混合模式的预处理弱阳离子交换固相萃取作为从生物样品中提取肽的有效方法。对于HRMS分析，选择全MS扫描采集模式以分别检测Dermorphin和Dermorphin（1-4）ATM / Z803.37226和457.20816的精确质量。 MS / MS确认协议中使用的SRM方法呈现出高特异性和灵敏度。 Dermorphin的所选产物离子为602.2,202.1和574.3，皮肤（1-4）为207.1,223.1和235.1。评估两种方法的特异性，可重复性，携带，矩阵效应和恢复。没有检测到残留和矩阵效应。初始测试程序的检测极限和确认程序的鉴定限度为2.5 ng / ml。此外，申请可以接受特异性和鲁棒性。在一起，开发方法证明是对人类兴奋剂控制目的的分析和代谢物的分析有效。

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