高效液相色谱法同时测定保健食品中9种非法添加降脂类药物

Simultaneous determination of 9 kinds of lipid lowering drugs illegally added in health food by high performance liquid chromatography

目的建立采用高效液相色谱法同时测定调节血脂类保健食品中烟酸、普伐他汀钠、瑞舒伐他汀钙、苯扎贝特、阿托伐他汀钙、氟伐他汀钠、吉非罗齐、洛伐他汀及辛伐他汀9种非法添加药物的方法。方法以甲醇为样品提取溶剂,采用Inertsil ODS-3色谱柱,以0.02 mol/L乙酸铵-甲醇为流动相梯度洗脱;流速为1.0m L/min;检测波长为230 nm,柱温为30℃,利用保留时间定性、外标法定量,分析9种非法添加药物。结果本方法可以在20 min内定性并定量分析烟酸、普伐他汀钠、瑞舒伐他汀钙、苯扎贝特、阿托伐他汀钙、氟伐他汀钠、吉非罗齐、洛伐他汀及辛伐他汀9种化学药物。9种非法添加药物在1.0-100μg/m L之间线性关系良好,相关系数均大于0.999;除阿托伐他汀钙在袋泡茶中回收率较低外,平均加标回收率范围为77.9%-102.9%,相对标准偏差范围为0.42%-5.8%。结论该方法线性关系良好,线性范围广,准确度及精密度高,可同时鉴定是否非法添加上述9种化学药物。

Objective To establish a method for the simultaneous determination of 9 kinds of drugs（nicotinic acid, pravastatin sodium, rosuvastatin calcium, bezafibrate, atorvastatin calcium, fluvastatin sodiu, gemfibrazil, lovastatin and simvastatin） illegally added in health food products for regulating blood lipid by high performance liquid chromatography（HPLC）. Methods The sample was extracted by methanol. A Inertsil ODS-3 chromatographic column was used with the mobile phase of 0.02 mol/L ammonium acetate-methanol for gradient elution, the flow rate was 1.0 m L/min, the detection wavelength was 230 nm, and the column temperature was 30 ℃. The 9 kinds of drugs were determined by the retention time, and quantified by the external standard method. Results The 9 kinds of drugs（nicotinic acid, pravastatin sodium, rosuvastatin calcium, bezafibrate, atorvastatin calcium, fluvastatin sodiu, gemfibrazil, lovastatin and simvastatin） could be analyzed qualitatively and quantitatively within 20 min. The drugs were detected at the range between 1.0 μg/m L and 100 μg/m L with good linearities, and the correlation coefficients were all greater than 0.999. Except for atorvastatin calcium in the teabag, the average recoveries were between 77.9% and 102.9%, and the relative standard deviations（RSDs） were 0.42%-5.8%. Conclusion The method has good linear relationships, wide linear ranges, high accuracy and precision, and can be used for the simultaneous determination of above 9 kinds of drugs.