中药产品中脱氢表雄酮和雄酮的检测。

Peng Zou, Ping Chen, Sharon Sze-Yin Oh, Kin-Har Kiang, Min-Yong Low
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引用次数: 4

摘要

采用气相色谱-质谱联用技术(GC-MS)和液相色谱-质谱联用技术(LC-MS/MS)检测中药制剂中脱氢表雄酮(DHEA)和雄酮(ADT)的含量。通过将DHEA和ADT的电子电离(EI)质谱与Wiley数据库中的电子电离(EI)质谱进行比较,初步鉴定了DHEA和ADT。采用液相色谱-质谱联用(LC-MS/MS)多反应监测(MRM)扫描,确认中药产品提取物中DHEA和ADT的存在。选择DHEA和ADT的[M + H]+和[M + NH4]+作为前体离子。DHEA的离子跃迁m/z为306.4 ~ > 271.2、306.4 ~ > 253.3、289.2 ~ > 270.9、289.3 ~ > 253.1,ADT的离子跃迁m/z为308.5 ~ > 273.6、308.5 ~ > 255.3、291.5 ~ > 273.5、291.5 ~ > 255.2,证实了两种类固醇激素的存在。在甲醇标准溶液中,选择脱氢表雄酮和ADT的[M +NH4]+为前体离子时,脱氢表雄酮和ADT的检出限分别为0.2 μ ml(-1)和0.3 μ ml(-1),可实现脱氢表雄酮和ADT的痕量检测,无需耗时衍生化。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Detection of dehydroepiandrosterone and androsterone in a traditional Chinese herbal product.

Dehydroepiandrosterone (DHEA) and androsterone (ADT) were detected in a traditional Chinese herbal product by gas chromatography-mass spectrometry (GC-MS) and liquid chromatography tandem mass spectrometry (LC-MS/MS). DHEA and ADT were tentatively identified by comparing their electron ionization (EI) mass spectra with those in the GC-MS Wiley database. A multiple reaction monitoring (MRM) scan was performed in LC-MS/MS to confirm the presence of the DHEA and ADT in the herbal product extract. Both the [M + H]+ and the [M + NH4]+ of DHEA and ADT were selected as the precursor ions. DHEA was detected with ion transitions m/z 306.4 --> 271.2, 306.4 --> 253.3, 289.2 --> 270.9, 289.3 --> 253.1 while ADT was detected with ion transitions m/z 308.5 --> 273.6, 308.5 --> 255.3, 291.5 --> 273.5, 291.5 --> 255.2, which confirmed the presence of the two steroid hormones in the herbal product. Limits of detection (LODs) of 0.2 microg ml(-1) for DHEA and 0.3 microg ml(-1) for ADT were found in methanolic standard solutions when [M +NH4]+ of DHEA and ADT were selected as the precursor ions, which allowed the detection of DHEA and ADT at trace level without time-consuming derivatization.

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