茯苓山药片中违法添加格列齐特和格列本脲的检测

Determination of Gliclazide and Glibenclamide Illegally Added into Poria Cocos Dioscorea Rhizoma Tablets by HPLC

目的:建立茯苓山药片中违法添加格列齐特和格列本脲的检测方法。方法:采用高效液相色谱法结合二级管阵列紫外光谱检测,色谱柱为SymmetryC18柱(4.6mm×250mm,5μm);流动相-A为水相(用磷酸调节pH值至3.5±0.1),流动相-B为乙腈进行梯度洗脱,流速:1mL/min,检测波长:230nm,柱温:35℃,进样量:10μL。结果:格列齐特与格列本脲的质量浓度分别在5.256～262.80μ/mL,2.890～144.50μg/mL范围内呈良好的线性关系;相关系数(r)、g平均回收率(%)与检测限分别为0.9998,101.29(n=9),1.0ng与0.9999,101.03(n=9),0.6ng。结论:本法具有良好的灵敏度和专属性,能对茯苓山药片中违法添加的格列齐特和格列本脲进行准确的定性和定量检测。

Objective：To establish a method for determination of gliclazide and glibenclamide illegally added into Poria cocos Dioscorea Rhizoma tablets by HPLC.Methods：A method of HPLC was established in which a diode-array detector was applied.The analysis was performed on Symmetry C18 column with column temperature set at 35 ℃,the mobile phase was composed of acetonitrile and aqueous solution which was adjusted to pH 3.5±0.1 with phosphate acid by gradient elution with a flow rate at 1 mL/min,and the injection volume was 10 μL.The detection wavelength was at 230nm.Results：The linear range of gliclazide was 5.256～262.80 μg/mL for assay,the average recovery was 101.29%（n = 9） and the detection limit was 1.0 ng.The linear range of glibenclamide was 2.890～144.50 μg/mL for assay,the average recovery was 101.03%（n = 9） and the detection limit was 0.6 ng.Conclusion：The method was highly sensitive and selective,and it can be used to detect gliclazide and glibenclamide illegally added into Poria cocos Dioscorea Rhizoma tablets accurately.