高效液相色谱-串联质谱检测保健酒中非法添加物艾地那非

Determination of Aildenafil Illegally Added in Health Wine by High Performance Liquid Chromatography- Tandem Mass Spectrometry

目的:采用高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)法,建立保健酒中非法添加物艾地那非的检测方法。方法:使用Agilent RRDH Eclipse-plus C18色谱柱(2.1 mm×100 mm,1.8μm),以0.1%甲酸-乙腈溶液为流动相A、0.1%乙酸-20 mmol/L乙酸铵溶液为流动相B进行梯度洗脱。通过HPLC-MS/MS系统中全扫描模式对艾地那非进行定性分析,多反应监测模式对艾地那非进行定量分析。结果:该方法线性r^2大于0.99,精密度相对标准偏差小于3%,不同质量浓度样品平均回收率为97.31%~100.66%,检出限为0.6 ng/m L,定量限为1.6 ng/m L。结论:此方法测定准确、灵敏度高、分离度高,可用于保健酒中非法添加物艾地那非的筛选和检测。

Objective： To develop a detection method for aildenafil adulterated in health wine using high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）. Methods： The chromatography was performed using an Agilent RRDH Eclipse plus C18 column（2.1 mm × 100 mm, 1.8 μm）, with a mobile phase consisting of acetonitrile-0.1%formic acid（phase A） and 0.1% acetic acid-20 mmol/L ammonium acetate（phase B） by gradient elution. Qualitative analysis of aildenafil was conducted under full-scan model, and quantitative analysis in the multiple reaction monitoring（MRM） model. Results： The method was linear with a correlation coefficient（r^2） 0.99, and its precision, expressed as RSD, was 3%. The recoveries of aildenafil at different spiked concentrations ranged from 97.31% to 100.66%. The limit of detection（LOD） was 0.6 ng/m L and the limit of quantitation（LOQ） was 1.6 ng/m L. Conclusion： This method is fast and accurate with a high sensitivity and a high degree of separation. It can be used for the screening and detection of aildenafil illegally added in health wine.