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

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

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50.0～5 000.0 μg/L,10.0～1 000.0 μg/L和40.0～4 000.0 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.

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 50.0-5000.0μg/L, 10.0-1000.0μg/L, 40.0-4000.0μg/L, with detection limits of 20.0, 4.0, 10.0μg/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.