便携式高效液相色谱仪的评价及其在同时检测保健食品中8种化学降糖药的应用

Evaluation of Portable High-performance Liquid Chromatography and Application for Detection of Eight Kinds of Anti-diabetic Agents in Health Care Products

评价实验室自行研制的便携式高效液相色谱仪的输液系统和整机性能,并应用于保健食品中8种化学降糖药的快速同时检测。实验采用ODS色谱柱(5μm,150 mm×4.6 mm),乙腈-0.02 mo.lL-1甲酸铵缓冲液(pH 3.8)(50:50)为流动相,检测波长229 nm。通过比较样品与对照品的保留时间,初步筛查样品中是否添加降糖化学成分,并将结果用液相色谱-质谱联用仪确认。结果显示该仪器的输液系统和整机性能均符合要求。8种化学降糖药在上述色谱条件下实现了完全分离,采用本文的方法实测了一批市售保健食品,检测出有格列本脲,LC-MS验证结果准确。格列本脲的线性范围为20～300 mg.mL-1(r=0.9986),平均回收率为100.3%。

The pumping system and overall performance of the portable high-performance liquid chromatography system developed by the laboratory is evaluated.It is applied to the detection of eight kinds of anti-diabetic agents in health care products.The separation was performed on Shim-pack VP-ODS（150 mm×4.6 mm,5 μm）,using the mixture of acetonitrile-0.02 mol.L-1ammonium（pH 3.8）（50：50） as the mobile phase.Detection wavelength was at 229 nm.The suspicious substances in the sample were screened out by comparing the peak retention time of a sample chromatogram with that of references possibly adulterated;then the suspicious substances were confirmed by LC-MS.The results showed that pumping system and overall performance meet the requirements.Eight kinds of compounds were well separated by this method.Glibenclamide was successfully detected in one batch of health care product,and the result was confirmed by LC-MS method.The linearity rang and average recovery for glibenclamide were 20-300 mg.mL-1（r=0.9986） and 100.3% respectively.