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
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10~200 μg/mL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/mL (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.
标题: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
英文标题:Detection of Illegally Added Thiovardenafil in Health-care Food Supplements by HPLC-MS
作者:
帅放文 湖南省药用辅料工程技术研究中心有限公司
王向峰 湖南省药用辅料工程技术研究中心有限公司
雷玉萍 湖南省药用辅料工程技术研究中心有限公司
肖江 湖南省药用辅料工程技术研究中心有限公司
汪修意 湖南省药用辅料工程技术研究中心有限公司;湖南尔康制药股份有限公司
中文关键词:硫代伐地那非,5型磷酸二酯酶,液相色谱-质谱联用,核磁共振,
英文关键词:thiovardenafil,iphophodiesterase 5,liquid chromatography-mass spectrometry,nuclear magnetic resonance,
发表日期:2015-10-24
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