液质联用法同时检测保健食品中非法添加的13种壮阳类化学品

Simultaneous determination of aphrodisiac compounds illegally added into health food by liquid chromatography-mass spectrometry

中文关键词:  保健食品  液相色谱-离子阱质谱法  壮阳

英文关键词:health food  liquid chromatography-ion trap mass spectrometry  aphrodisiac

中文摘要:

      目的 建立同时检测保健食品中非法掺入13种壮阳类化学品的液质联用方法, 并对100批市售样品进行检测。方法 采用液相色谱-离子阱质谱法对样品进行检测, 样品经甲醇超声提取、C18色谱柱分离, 以甲醇-乙腈-20 mmol/L乙酸铵溶液为流动相, 进行梯度洗脱。在电喷雾离子化正离子和负离子模式下, 以一级全扫描和二级全扫描模式检测, 扫描范围为50~1000 u。结果 13种化合物的检出限为0.1~5 ng, 在100批样品中, 5批检测出西地那非, 2批检测出他达拉非, 1批检测出硫代西地那非。结论 该法选择性强, 灵敏度高, 可以用于分析检测保健食品中是否掺入壮阳类化学品。

英文摘要:

      Objective To establish a method for simultaneous determination of aphrodisiac compounds illegally added into health food by liquid chromatography-ion trap mass spectrometry method, and detect 100 batches of commercial samples. Methods The samples were detected by liquid chromatography-ion trap mass spectrometry. Samples were ultrasonically extracted with methanol, separated on a C18 column with mobile phase of methanol-acetonitrile-20 mmol/L ammonium acetate solution for gradient elution. The samples were detected by electrospray ion source in positive and negative modes with full MS and full scan MS2 modes. The scan rang was 50-1000 u. Results The limits of detection for 13 compounds were 0.1-5 ng. Sildenafil was found in 5 samples, tadalafil was found in 2 samples and thiosildenafil was found in 1 sample. Conclusion The method is selective and sensitive, which can be used to detect the aphrodisiac compounds illegally added into health food.