OBJECTIVE: To improve the detection method for the dissolution of dihydroartemisinin in Dihydroartemisinin and piperaquine phosphate tablets. METHODS: The dissolution experiment adopted paddle method using 0.1 mol/L hydrochloric acid solution 500 mL as solvent with rotating speed of 75 r/min and sampling time of 45 min. In sample pre-treatment, the volume of 3.6% sodium hydroxide solution was increased from 5 mL to 20 mL, and that of phosphoric acid was increased from 0.2 mL to 0.7 mL. HPLC was adopted to determine the dissolution of dihydroartemisinin. The determination was performed on YMC-Pack ODS-A column with mobile phase consisted of 0.02 mol/L disodium hydrogen phosphate solution(pH adjusted to 2.4 using phosphoric acid)-acetonitrile (65 ∶ 35,V/V) at the flow rate of 1.0 mL/min. The detection wavelength was set at 237 nm,and column temperature was 30 ℃. The sample size was 20 μL. RESULTS: The linear range of dihydroartemisinin were 7.802-117.03 μg/mL(r=0.999 9). The limit of quantitation was 2.0 ng, and the limit of detection was 0.6 ng. RSDs of precision and reproducibility tests were all lower than 1.0%. The recoveries were 99.18%-100.46% (RSD=0.45%,n=9). Average dissolutions of dihydroartemisinin in 3 batches of samples were 94.9%, 77.9%, 89.6%, respectively. CONCLUSIONS: Improved method enhance the accuracy for the limit of sensitivity, dissolution and detection results.
关键词
双氢青蒿素哌喹片双氢青蒿素溶出度测定方法改进
Keywords
Dihydroartemisinin and piperaquine phosphate tabletsDihydroartemisininDissolution determinationMethod improvement