色谱

色谱

• 研究简报 • 上一篇    下一篇

高效液相色谱-质谱法测定性保健品中脱水吗啡、西地那非、前列地尔

徐远金1,2,许桂苹1

  

  1. 1. Engineering Center for Sugar Cane and Cane Sugar, Guangxi University, Nanning 530004, China; 2. Guangxi Key Laboratory of Subtropical Bioresource Conservation and Utilization, Guangxi University, Nanning 530004, China
  • 收稿日期:2004-10-14 修回日期:1900-01-01 出版日期:2005-11-30 发布日期:1987-12-25
  • 通讯作者: 徐远金

Determination of Apomorphine, Sildenafil and Alprostadil in Medicines for Erectile Dysfunction by High Performance Liquid Chromatography-Mass Spectrometry

XU Yuanjin1,2, XU Guiping1   

  1. 1. Engineering Center for Sugar Cane and Cane Sugar, Guangxi University, Nanning 530004, China; 2. Guangxi Key Laboratory of Subtropical Bioresource Conservation and Utilization, Guangxi University, Nanning 530004, China
  • Received:2004-10-14 Revised:1900-01-01 Online:2005-11-30 Published:1987-12-25

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摘要：

建立了高效液相色谱-电喷雾电离质谱法同时测定性保健品中违禁药物脱水吗啡、西地那非和前列地尔的分析方法。样品用甲醇超声提取,用Zorbax Eclipse XDB-C18柱分离,以乙腈-0.5%甲酸水溶液作为流动相,以保留时间和质荷比对分离出的组分予以定性确证,用峰面积进行定量。结果表明,脱水吗啡、西地那非和前列地尔的线性范围分别为50.0~5000.0 μg/L,10.0~1000.0 μg/L和40.0~4000.0 μg/L,检出限(以信噪比为3计)分别为20.0,4.0和10.0 μg/L。样品的加标平均回收率为89%~95%,相对标准偏差为9.5%~11%。该方法简便、快速、灵敏,适用于含中药成分的性保健品中这3种药物的同时分析。

关键词: 高效液相色谱-质谱法, 前列地尔, 脱水吗啡, 西地那非, 性保健品

Abstract:

A high performance liquid chromatography-mass spectrometry (LC-MS) analytical method for illicit drugs, apomorphine, sildenafil and alprostadil, in medicines for erectile dysfunction has been developed. The samples were extracted with methanol using ultrasound-assisted extraction. The chromatographic separation was performed on a Zorbax Eclipse XDB-C18 column using acetonitrile-0.5% formic acid aqueous solution as mobile phase. The three compounds were identified by retention time and m/z and quantified by peak area. The results demonstrated that the linear ranges were 50.0-5000.0 μg/L, 10.0-1000.0 μg/L, 40.0-4000.0 μg/L, with detection limits of 20.0, 4.0, 10.0 μg/L for apomorphine, sildenafil and alprostadil, respectively. The average recoveries and the relative standard deviations were 89%-95% and 9.5%-11%. The method is simple, rapid, accurate and suitable for the simultaneous determination of these drugs in medicines for erectile dysfunction.

Key words: alprostadil, apomorphine, medicines for erectile dysfunction , sildenafil, high performance liquid chromatography-mass spectrometry