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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 establish a liquid chromatography-mass spectrometry (HPLC-MS) method for the detection of illicit incorporation of thio-dinafil into health products. Methods The samples of health care products were extracted by ultrasonic extraction of methanol and analyzed by liquid chromatography-tandem quadrupole mass spectrometry. According to the relative molecular weight, the retention time of chromatographic liquid chromatography and the area of chromatographic peaks, Vardenafil for qualitative and quantitative analysis. Results In the concentration range of 10 ~ 200μg / mL, there was a good linear relationship between the concentration of thio - vardenafil and the peak area, r2 = 0.998. The precision and stability were good. The average recovery was 99.9% and the RSD was 0.613 %, The method is accurate and reliable, the specificity is strong, and the content of thio-daldenafil measured in a commercially available health product is 0.34%. Conclusions Liquid chromatography-mass spectrometry (LC-MS / MS) method is highly specific and sensitive and can be used as an effective method for the detection of illicit incorporation of thio-dinafilofetil in health products.