HPLC－DAD法测定复方麻黄散中非法添加喹烯酮

Determination of Quincetone Added illegally to Fufang Mahuang San by HPLC-DAD

关键词:  HPLC－DAD法  复方麻黄散  喹烯酮  非法添加

Key words:  HPLC－DAD  Fufang Mahuang San  Quincetone  illegal addition

摘要:

建立了复方麻黄散中非法添加喹烯酮的HPLC－DAD检查方法。以C18柱为固定相，甲醇－水（60:40，V:V）为流动相，流速为1.0 mL/min，柱温30℃，二极管阵列检测器检测，采集波长范围为190~400nm，提取波长为314 nm。通过液相色谱保留时间、紫外吸收光谱和峰纯度分析对非法添加物进行确认。结果表明，该色谱条件下喹烯酮与其他物质分离良好。喹烯酮在2.0~100.0 μg/mL范围内线性关系良好，R2=0.9999。喹烯酮在复方麻黄散中的平均回收率为101.4%，RSD为0.5%；方法的检测限为0.25 g/kg。该方法简便，准确，可靠，可以用于检查复方麻黄散中非法添加喹烯酮。

Abstract:

A method for determining quincetone Added illegally to Fufang Mahuang San was established by the high performance liquid chromatography with photo-diode array detector (HPLC-DAD). It was tested using C18 column as stationary phase and methanol-water (60:40, V:V) as mobile phase; the detection wavelength was 314 nm, while acquiring wavelength were between 190 nm and 400 nm; the flow rate was 1.0mL/min; the column temperature was 30℃. The quincetone was detected and verified with similar retention time and spectrum, and good peak purity. Result showed that the quincetone was separated finely with other materials under the chromatographic condition. When concentration of reference quincetone solutions were in the range of 2.0~100.0 μg/mL, the linear relationship was good, with R2=0.9999. The average recovery of quincetone was 101.4%, with RSD of 0.5%, and the detection limit was 0.25 g/kg. The method is simple, accurate and reliable for determining quincetone added illegally to Fufang Mahuang San.