Abstract:
OBJECTIVE To establish an optimum preparation technology and the method for quality control of Xuanshen dripping pills.
METHODS Orthogonal test was applied to optimize the preparation with the choice of substrate, its proportion of substrate to drug, the drug and refrigerant temperature, dropping speed and distance to make dissolution time, appearance and weight variation up to grade. Using TLC to identify the dripping pills, harpagoside in dripping pills was determined by UPLC. Using ACQUITY UPLC BEH C
18 column (2.1 mm×100 mm, 5 μm), the mobile phase was acetonitrile-1% ethylic acid (31∶69), the column temperature was 35 ℃, the flow rate was 0.2 mL·min-1 and the detection wavelength was 278 nm.
RESULTS The optimum pills preparation was the ratio of PEG4000 to PEG6000 (4∶1) and drug to substrate (1∶3). Drug temperature was 90 ℃. The mixed liquid of dimethicone and liquid paraffin was refrigerant. Drug was dropped into the refrigerant of 0 ℃ by (20±2) dropping per minute (freeze-pillar height 3 cm). The herbs could be identified by TLC. For harpagoside, the linear range was 0.010-0.040 μg(
r=0.999 9), and the average recovery was 99.2%, RSD was 0.87%.
CONCLUSION The good quality pills can be produced through this process with the simple and reliable method. The determination method is simple, specific, reproducible and accurate, and can be applied to the quality control for the Xuanshen dripping pills.