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使用电子电离和化学电离的低成本质谱检测器对不同去甲雄酮衍生物进行质谱表征。

Mass spectrometric characterization of different norandrosterone derivatives by low-cost mass spectrometric detectors using electron ionization and chemical ionization.

作者信息

de Boer D, de Jong E G, Maes R A

机构信息

Netherlands Institute for Drugs and Doping Research, State University of Utrecht.

出版信息

Rapid Commun Mass Spectrom. 1990 Jun;4(6):181-5. doi: 10.1002/rcm.1290040604.

Abstract

The abuse of nortestosterone in sport is an important problem in doping-control analysis. In order to detect the main urinary metabolite of nortestosterone, norandrosterone (NA), sensitive and specific methodology is necessary. In this context the use of a low-cost mass spectrometric detector such as the Finnigan MAT ion-trap detector (ITD) was studied. The electron ionization (EI) and positive-ion chemical ionization (PICI) mass spectra of the methoxime-trimethylsilyl, trimethylsilyl-enol trimethylsilyl ether and pentafluoropropionic ester derivatives of NA are described. The limits of detection of these derivatives are compared with those obtained by the Hewlett-Packard mass selective detector (MSD), another low-cost mass spectrometric detector and operating only in the EI mode. For the derivatives of the reference standard of NA the ITD has in the EI mode the same limit of detection, in the range of 0.5 to 1 ng injected on the column, as the MSD. However, under these conditions the ITD provides more spectrometric information, because it gives full scan data. Moreover, with the same or even improved limits of detection the ITD can operate in the PICI mode. On the other hand, for the analysis of NA isolated from urine samples, the performance of the MSD was better than that of the ITD. The ion trapping technique is probably limited when the chemical background is high.

摘要

在运动中滥用诺龙是兴奋剂检测分析中的一个重要问题。为了检测诺龙的主要尿液代谢物去甲雄酮(NA),需要灵敏且特异的方法。在此背景下,研究了使用如菲尼根MAT离子阱检测器(ITD)这样的低成本质谱检测器。描述了NA的甲氧肟 - 三甲基硅烷基、三甲基硅烷基 - 烯醇三甲基硅烷基醚和五氟丙酸酯衍生物的电子电离(EI)和正离子化学电离(PICI)质谱。将这些衍生物的检测限与通过惠普质量选择检测器(MSD)获得的检测限进行比较,MSD是另一种低成本质谱检测器,且仅在EI模式下运行。对于NA参考标准品的衍生物,在EI模式下,ITD的检测限与MSD相同,在柱上进样0.5至1 ng的范围内。然而,在这些条件下,ITD能提供更多的光谱信息,因为它能给出全扫描数据。此外,在检测限相同甚至有所改善的情况下,ITD可以在PICI模式下运行。另一方面,对于从尿液样本中分离出的NA的分析,MSD的性能优于ITD。当化学背景较高时,离子阱技术可能会受到限制。

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