Optimization of the Quality Control Method of Qingkailing Dropping Pills
YAN Hai-xia, FU Xin-tong, CHEN You-gen, GUO Hong-zhu, CHANG Zeng-rong*
Beijing Center for Health Food and Cosmetics Control, Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine, Beijing Institute for Drug Control, Beijing 102206, China
Abstract：OBJECTIVE To optimize and improve the quality standard of Qingkailing dropping pills. METHODS Lonicerae Japonicae Flos, geniposide in Gardeniae Fructus and baicalin in Scutellariae Radix of Qingkailing dropping pills were identified by TLC and HPLC respectively. Cholic acid and hydrodeoxycholic acid were determined by HPLC equipped with an ELSD and a column (4.6 mm×250 mm, 5 μm) packed with ODS bonded silica gel (5 μm particle size). The mobile phase was a mixture of methanol, acetonitrile and 0.1% formic acid (68∶17∶15, V/V/V) and the flow rate was 1.0 mL·min-1. Geniposide in Gardeniae Fructus of Qingkailing dropping pills was determined by HPLC equipped with a DAD (238 nm) and a column (4.6 mm×250 mm) packed with ODS bonded silica gel (5 μm particle size). The mobile phase was a mixture of acetonitrile and 0.05% phosphoric acid (10∶90, V/V) and the flow rate was 1.0 mL·min-1. Baicalin in Scutellariae Radix of Qingkailing dropping pills was determined by HPLC equipped with a DAD (275 nm) and a column (4.6 mm×150 mm) packed with ODS bonded silica gel (5 μm particle size), the mobile phase was a mixture of methnol, water and phosphoric acid (47∶53∶0.2, V/V/V), and the flow rate was 1.0 mL·min-1. RESULTS The developed TLC spots were clear with good reproducibility. Hydrodeoxycholic acid, cholic acid, geniposide and baicalin showed good linear relationship in the ranges of 0.505 0-6.312 μg, 0.515-6.440 μg, 0.029 12-0.582 4 μg, and 0.109 2-1.092 μg, respectively. The average recoveries (n=6) were 101.5%, 101.6%, 98.61% and 99.77%, with RSDs of 1.7%, 1.5%, 1.42% and 0.79%, respectively. CONCLUSION The method is simple, rapid, accurate, with low toxicity, and can be used to control the quality of Qingkailing dropping pills more effectively and comprehensively.
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2020, Vol. 55 
