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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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甲基屈他雄酮在人体内的代谢产物研究

Analysis of methasterone in human urine by gas chromatography-mass spectrometry

分类号:R917
出版年·卷·期(页码):2020,40 (4):644-650
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的: 研究口服甲基屈他雄酮(methasterone)后人尿中代谢产物的情况。方法: 招募健康志愿者口服甲基屈他雄酮100 mg,收集服药前空白尿样,服药后72 h内全部尿样,以及第4至20天晨尿。尿样经过酶解、液-液萃取、衍生化等前处理步骤,采用GC/MSD-MS和GC-MS/MS检测尿样中甲基屈他雄酮及代谢产物,并研究其在人尿中的代谢情况。色谱-质谱条件:HP-1毛细管色谱柱(25 m×0.2 mm×0.11 μm),柱温为程序升温(起始温度177℃,以3℃·min-1的速率升至245℃,然后以17℃·min-1的速率升至320℃,保持2.5 min),载气为高纯氦气,进样口温度280℃,柱压138 kPa,分流比10:1,进样量2 μL;质谱离子源为EI源,源温度230℃,电子能量70 eV,采集模式为Scan(m/z 40~700)和MRM。结果: 研究结果表明,口服甲基屈他雄酮在人尿中的以原型甲基屈他雄酮及C3位羟基化还原产物为主,这2种物质是目前兴奋剂检测领域检测甲基屈他雄酮摄入的目标物质。结论: 通过对口服甲基屈他雄酮在人尿中代谢产物的研究,发现可作为辅助检测甲基屈他雄酮摄入的代谢产物M2~M4,通过对多种代谢物信息综合研判,可降低假阳性风险,提高兴奋剂检测的可靠性、科学性。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To investigate the metabolic profile of methasterone in human urine after oral administration of methasterone. Methods: A male volunteer orally took a single dose of 100 mg methasterone substance. Urine blank was collected before administration,and then all urine excreted within 72 hours after administration were collected. From day 4 to 20,the morning urines were also collected. The urine samples were pre-treated using enzymatic hydrolysis,liquid-liquid extraction and derivation and then examined by GC/MSD-MS and GC-MS/MS to detect methasterone and its metabolites and investigate metabolic profile of methasterone. Analytical parameters:a HP-1 cross-linked capillary column(25 m×0.2 mm×0.11 μm) was adopted,the initial column temperature was set at 177℃ and then increased at a rate of 3℃·min-1 to 245℃ and continue to increase to 320℃ at a rate of 17℃·min-1 to and then holding for 2.5 min;the transfer line temperature was maintained at 280℃,and the column pressure was 138 kPa;the split ratio was 10:1,with 2 μL injection volume;the electronsource temperature was 230℃ with electron energy of 70 eV;Data were obtained in Scan (m/z 40 to 700) and multiple reaction monitoring(MRM) mode. Results: This study found that methasterone and the C3 hydroxylated reduzate were the major metabolites of methasterone in human urine,which were now the target compounds to determine methasterone abuse in doping detection. Conclusion: The findings of this study suggested that M2-M4 metabolites could be as the auxiliary markers to enhance the reliability of methasterone determination and reduce the possibility of false positive results.

-----参考文献:---------------------------------------------------------------------------------------
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