液相色谱－串联质谱法同时测定保健食品中 四种违禁药物含量

Simultaneous determination of 4 kinds of illicit drugs in health-care foodstuffs by ultra performance liquid chromatography-mass spectrometry

中文关键词:  超高效液相色谱-串联质谱  保健食品  西地那非  他达那非  伐地那非  红地那非

英文关键词:Ultra performance liquid chromatography-mass  health-care foodstuffs  Sildenafil  Tadalafil  Vardenafil  Acetildenafil

中文摘要:

      目的　建立超高效液相色谱-串联质谱法测定保健食品中西地那非、他达那非、伐地那非以及红地那非四种违禁药物含量的方法。方法 采用ACQUITY UPLC BEH C18(100 mm×2.1 mm, 1.7 μm)色谱柱, 以甲醇和添加0.1%甲酸5 mmol乙酸铵为流动相, 梯度洗脱程序, 进样分析20 min, 在电喷雾正离子模式下以多反应监测(MRM)方式检测, 外标法定量。结果 四种那非类违禁药物的检出限(LOD, S/N=3)和定量限(LOD, S/N=10)分别0.1~0.5 μg/kg和0.3~2.0 μg/kg在0.1~100 μg/kg浓度范围内线性关系良好(r>0.99), 加标回收率为73.6%~90.4%, 相对标准偏差为1.0~8.9。结论 该方法操作简单, 重现性好, 背景噪音低, 具有较高的灵敏度和选择性。

英文摘要:

      Objective To develop a method for the simultaneous determination of　sildenafil, tadalafil,　vardenafil and acetildenafil　in health-care foodstuffs by ultra performance　liquid chromatography-mass　spectrometry. Methods　The elution was separated on an ACQUITY UPLC BEH C18 column(100 mm×2.1 mm, 1.7 μm) using the methanol -5 mmol ammonium acetate containing 0.1% formic acid　as the mobile phase and a gradient elution program with a cycle time of 20 min, detected by electrospray ionization mass spectrometry in positive mode with multiple reaction monitoring, quantified by external standard method. Results The limits of detection(LOD, S/N=3)and quantification(LOQ, S/N=10) of 4 compounds were 0.1~0.5 μg/kg and 0.3~2.0 μg/kg, respectively. The correlation coefficients of linear calibration curve were over 0.99 in the ranges of 0.1~100 μg/kg. Average fortified recoveries were 73.6%~90.4%, and the relative standard deviations were in the ranges of 1.0~7.9. Conclusion This method has the advantages of simple operation, good reproducibility, low background noise, higher sensitivity and selectivity.