液联用法检测保健食品和中成药中10种壮阳类违禁药物

摘要

本实验建立了超高效液相色谱-串联质谱法同时测定保健食品和中成药中10种壮阳类违禁药物(磷酸二酯酶-5型抑制剂类)的分析方法.采用甲醇提取样品中的被测物质,BEH C18柱分离,以乙腈-10mmol/L甲酸铵+0.1％甲酸水为流动相,梯度洗脱;质谱条件是采用电喷雾正离子扫描(ESI+),多反应监测(MRM)模式.结果表明,标准溶液在0.1～20ng/mL浓度范围内,线性良好,相关系数(R2＞0.99).保健食品、中成药和药酒三种基质的加标回收率范围62.3～102.5％,精密度范围0.67～15.38％ (RSD,n=4),方法稳定可靠.本方法适用于同时测定中成药、保健食品和药酒中10种壮阳类违禁药物.%A method was developed for simultaneous determination of 10 illegal added anti-impotence medicines (phosphodiesterase-5 inhibitors) in health foods and Chinese proprietary medicine samples by UPLC-MS/MS.Samples were extracted by methanol,the extracts were separated by BEH C18 column,using acetonitrile and 10 mmol/L ammonium acetate water solution containing 0.1％ acetic acid as the mobile phase with gradient elution.The compounds were detected by positive electrospray ionization-tandem mass spectrometry (ESI+) in multiple reaction monitoring (MRM) mode.As the result,in the range of 0.1～20ng/mL,the correlation coefficient was above 0.99 (R2＞0.99);the average recoveries of 10 target compounds in spiked health foods,Chinese proprietary medicine and health wine samples were 62.3～102.5％;the relative standard deviations (RSD,n=4) were 0.67～15.38％.This method is suitable for determination of 10 illegal added anti-impotence medicines in health foods and Chinese proprietary medicine samples.