液相色谱-质谱联用法检测保健品中非法掺入的硫代伐地那非

Detection of illegally added thiovardenafil in healthcare foods by liquid chromatography-mass spectrometry

目的建立保健品中非法掺入硫代伐地那非的液相色谱-质谱联用法(HPLC-MS)检测方法。方法保健品样品经甲醇超声提取得提取液,用液相色谱-串联四极杆质谱进行分析,根据相对分子量、液相色谱保留时间、色谱峰面积等,对保健品中非法掺入的硫代伐地那非进行定性以及定量分析。结果在10~200μg/m L浓度范围内,硫代伐地那非浓度与峰面积呈良好线性关系,r2=0.998,精密度和稳定性良好,加样平均回收率为99.9%,RSD为0.613%,方法准确可靠,专属性强,并测得某市售保健品中硫代伐地那非的含量为0.34%。结论液相色谱-质谱联用法专属性强,灵敏度高,可作为检测保健品中非法掺入硫代伐地那非的有效方法。

Objective To develop a high performance liquid chromatography-mass spectrometry(HPLC-MS) method for the identification of illegally added thiovardenafil in healthcare foods. Methods Thiovardenafil in healthcare food was extracted with methyl and then analyzed by HPLC-MS. Qualitative and quantitative analysis were conducted according to relative molecular weight, retention time and peak aera. Results Good linearly correlation were detected in the range of 10 to 200 μg/m L(r2=0.998, n=5). The average recovery rate was 99.9%, and RSD was 0.613%(n=6). The content of thiovardenafil the in a market sample was 0.34%. Conclusion The method is selective and sensitive, which can be used to detect thiovardenafil illegally added in healthcare food suplements.