HPLC-MS/MS法同时检测抗疲劳药物及保健品中非法添加的7种壮阳类化学药物

Simultaneous Detection of 7 Illegal Added Anti-impotence Medicines in Anti-fatigue Preparations and Health Care Products by HPLC-MS/MS

目的:建立检测抗疲劳药物及保健品中非法添加的7种壮阳类化学药物的方法。方法:采用高效液相色谱-质谱串联(HPLC-MS/MS)法。色谱柱:Acclaim120C18,流动相:甲醇-0.01mol/L醋酸铵溶液(35:65,V/V),流速:0.2ml/min,选择正离子多反应监测扫描方式检测,离子通道分别为质荷比(m/z)475.2→100.1(枸橼酸西地那非)、m/z489.5→151.1(伐地那非)、m/z467.4→111.1(红地那非)、m/z453.0→112.9(那红地那非)、m/z489.6→283.3(豪莫西地那非)、m/z505.4→487.3(羟基豪莫西地那非)、m/z355.3→144.1(育亨宾)。结果:枸橼酸西地那非、伐地那非、红地那非、那红地那非、豪莫西地那非、羟基豪莫西地那非与育亨宾的检测质量浓度的线性范围分别为2.0～200.0(r=0.9992)、0.5～100.0(r=0.9996)、1.0～100.0(r=0.9995)、1.0～100.0(r=0.9999)、2.0～200.0(r=0.9999)、0.5～100.0(r=0.9996)、1.0～100.0ng/m(lr=0.9992),检测限分别为2.0、0.5、1.0、1.0、2.0、0.5、1.0ng/ml,平均回收率分别为98.1%、99.0%、97.8%、100.3%、99.6%、98.4%、97.5%,RSD均<4%(n=6)。结论:本方法能够快速、准确地检测出抗疲劳药物及保健品中非法添加的7种壮阳类化学药物。

OBJECTIVE： To establish a method for the determination of 7 illegal added anti-impotence medicines in anti-fatigue preparations and health care products. METHODS： HPLC-MS/MS method was adopted. The determination was performed on Acclaim 120 C18 column with mobile phase consisted of methanol-0.02 mol/L ammonium acetate （35 ： 65, V/V） at the flow rate of 0.2 ml/min. The mass transition pairs of m/z 475.2→200.1 （sildenafil citrate）, m/z 489.5→151.1 （vardenafil）, m/z 467.4→111.1 （hongdenafil）, m/z 453.0→112.9 （nor-acetylsidenafil）, m/z 489.6→283.3 （homosildenafil）, m/z 505.4→487.3 （hydroxyhomosilde- nafil）, m/z 355.3→144.1 （yuhimbine） were used to detect the 7 kinds anti-impotence preparations under positve ion multiple reac- tion monitoring mode. RESULTS： The linear ranges were 2.0-200.0 ng/ml for sildenafil citrate （r=0.999 2）, 0.5-100.0 ng/ml for vardenafil （r=0.999 6）, 1.0-100.0 ng/ml for hongdenafil （r=0.999 5）, 2.0-100.0 ng/ml for nor-acetylsidenafil （r=0.999 9）, 2.0- 200.0 ng/ml for homosildenafil （r=0.999 9） , 0.5-100.0 ng/ml for hydroxyhomosildenafil （r=0.999 6） and 1.0-100.0 ng/ml for yuhimbine （r=0.999 2）. The lowest limits of detection were 2.0 ng/m2, 0.5 ng/ml, 1.0 ng/ml, 2.0 ng/ml, 2.0 ng/ml, 0.5 ng/ml and 1.0 ng/ml, respectively. Average recoveries were 98.1%, 99.0%, 97.8%, 100.3%, 99.6%, 98.4% and 97.5% （RSD〈4%, n = 6）. CONCLUSIONS ： The method is quick and accurate for the determination of 7 illegal added anti-impotence medicines in an- ti-fatigue preparations and health care products.