高效液相色谱检测中成药及保健品中非法添加14个降血脂类化学药物的研究

Simultaneous determination of fourteen hypolipidemic drugs illegally adulterated in Chinese patent medicines and health foods by HPLC

目的:应用高效液相色谱(HPLC)技术,建立降血脂类中成药及保健品中可能添加的普伐他汀钠、瑞舒伐他汀钙、苯扎贝特、依折麦布、吉非贝齐、洛伐他汀、氯贝丁酯、辛伐他汀、非诺贝特、普罗布考、烟酸、阿昔莫司、氟伐他汀钠、阿托伐他汀钙的检查方法。方法:采用Shimadzu C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸水溶液,梯度或等度洗脱,流速1.0 mL·min^-1或0.8 mL·min^-1,柱温30℃,检测波长230、236、246 nm。结果:14个化学药物在一定质量浓度范围内与峰面积呈良好的线性关系;回收率良好,低、中、高3个浓度的平均回收率(n=9)为99.1%~100.1%,RSD为0.86%~1.3%;精密度良好,RSD均小于0.70%;稳定性良好,14个成分在24 h内保持稳定,RSD均小于1.0%。利用本法,从13批样品中检出1批非法添加化学药物。结论:该方法简便、准确、快速,易于推广,可作为中成药及保健品中非法添加14个降血脂类化学药物的检查方法。

Objective:To develop the high-performance liquid chromatography(HPLC)method for detection of pravastatin sodium,rosuvastatin calcium,benzafibrate,ezetimibe,gemfibrozil,lovastatin,clofibrate,simvastatin,fenofibrate,probucol,nicotinic acid,acipimox,fluvastatin sodium and atorvastatin calciumillegally adulterated in Chinese patent medicines and health foods.Methods:An Shimadzu C18 column(250 mm×4.6 mm,5μm)was used for the separation,with gradient elution or isocratic elution of acetonitrile and 0.1%phosphoric acid as the mobile phase at a flow rate of 1.0 mL·min^-1 or 0.8 mL·min^-1.The detection wavelength was set at 230,236 and 246 nm.The column temperature was 30℃.Results:Fourteen chemical constituents showed good linearity within certain concentration ranges.The average spiked recoveries(n=9)of low,middle and high levels ranged from 99.1%to 100.1% and RSDs were 0.86%-1.3%.The precision was satisfactory with all RSDs below 0.70%.The stability within 24 h was satisfactory with the RSDs below 1.0%.Using this method,one batch of illegally adulterated chemical substance was detected from thirteen batches of samples.Conclusion:The established method is simple,accurate,fast and propagable for the detection of fourteen hypolipidemic drugs illegally adulterated in Chinese patent medicines and health foods.