超高效液相色谱-串联质谱法测定抗疲劳类保健食品及补肾壮阳类中成药中15种添加药物

目的：建立一种测定补肾壮阳类中成药及抗疲劳类保健食品中15种非法添加药物的超高效液相-串联质谱（UPLC-MS/MS）方法。方法：样品经甲醇超声提取后，采用Thermo C₁₈色谱柱（100 mm×2.1 mm，1.9 μm）分离，以含0.1%甲酸的乙腈-含0.1%甲酸的10 mmoL·L^-1乙酸铵为流动相，梯度洗脱，多反应监测测定15种非法添加药物（达那唑、司坦唑醇、甲磺酸酚妥拉明、甲睾酮、豪莫西地那非、枸橼酸羟基豪莫西地那非、硫代艾地那非、那莫西地那非、伪伐地那非、盐酸育亨宾、氨基他达拉非、西地那非、他达拉非、盐酸伐地那非、丙氧苯基-硫代羟基豪莫西地那非）。结果：15种非法添加药物在2.7~679 ng·mL^-1范围内线性关系良好，相关系数（r²）均大于0.995，平均回收率70%~120%。所检26批样品中9批检出西地那非、1批检出丙氧苯基-硫代羟基豪莫西地那非，阳性率为38%。结论：本方法准确，灵敏度高，专属性好，检测限低，可用于中成药及保健食品中15种非法添加药物的定性及定量测定。

Objective:To establish an UPLC-MS/MS method for simultaneous determination of 15 illegal additives in invigorant Chinese patent medicines and antifatigue dietary supplements.Methods:After ultrasonic extracted by methanol,the sample was separated on Thermo C₁₈(100 mm×2.1 mm,1.9 μm)column with gradient elution.The mobile phase consisted of acetonitrile containing 0.1% formic acid^-10 mmoL·L^-1 ammonium acetate containing 0.1% formic acid at a flow rate of 0.2 mL·min^-1.Multiple reactions monitoring mode was used to quantify the 15 illegally added additives(danazole,stanzolol,phentolamine mesylate,methyltestosterone,homosildenafil,hydroxyhomosildenafil,thioaildenafil,namosidenafil,pseudovardenafil,vardenafil,yohimbine hydrochloride,amino tadalafil,sildenafil,tadalafil,vardenafil hydrochloride and propoxyphenyl-thiohydroxyhomosil).Results:15 illegal additives had good linear relationship in the range of 2.7-679 ng·mL^-1 with correlation coefficients(r²)above 0.995,and the average recoveries were 70%-120%.Sildenafil was detected in 9 batches and propoxyphenyl-thiohydroxysildenafil was detected in 1 batch out of 26 samples.The positive rate was 38%.Conclusion:This method is accurate,sensitive,specific with low detection limit.It can be used for the qualitative and quantitative determination of 15 illegal additives in Chinese patent medicines and dietary supplements.

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