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目的:建立HPLC测定白头翁总皂苷乳剂中白头翁皂苷B3及白头翁皂苷BD含量的方法,测定该乳剂体外释放度。方法:采用液液萃取法处理样品,HPLC进行检测。色谱条件为Diamonsil C18色谱柱(4.6 mm×250 mm,5μm),C18保护柱(4.0 mm×3.0 mm),柱温40℃,流动相乙腈-水-四氢呋喃(52∶45∶3),流速1.0 mL·min-1,检测波长203 nm,进样量10μL。采用改良的动态透析法进行白头翁总皂苷乳剂及白头翁总皂苷水溶液的体外释药试验。结果:白头翁皂苷B3和白头翁皂苷BD的线性范围分别为0.01～1(r=0.999 6),0.01～2(r=0.999 8)g·L-1,精密度的RSD分别为3.19%,1.17%,重复性RSD分别为1.40%,1.60%,平均回收率分别为99.63%,100.27%。3批白头翁总皂苷乳剂中白头翁皂苷B3质量浓度分别为0.186,0.190,0.191 g·L-1,白头翁皂苷BD分别为0.069,0.065,0.066 g·L-1。该乳剂中白头翁皂苷B3及白头翁皂苷BD在pH 7.4磷酸盐缓冲液中12 h的累积释放率分别91.30%,74.97%。结论:建立的方法准确、灵敏,适用于白头翁乳剂指标成分含量及释放度的测定。
OBJECTIVE: To establish a HPLC method for the determination of Pulsatilla saponin B3 and Pulsatilla saponin BD in Pulsatilla saponin emulsion and to determine its in vitro release. Methods: Samples were processed by liquid-liquid extraction and detected by HPLC. The chromatographic conditions were Diamonsil C18 column (4.6 mm × 250 mm, 5 μm), C18 guard column (4.0 mm × 3.0 mm), column temperature 40 ℃, mobile phase acetonitrile-water-tetrahydrofuran mL · min-1, detection wavelength of 203 nm, injection volume of 10μL. A modified dynamic dialysis method for Pulsatilla saponin emulsion and Pulsatilla total saponin aqueous solution in vitro release test. RESULTS: The linear ranges of Pulsatilla saponin B3 and Pulsatilla saponin BD were 0.01-1 (r = 0.999 6) and 0.01-2 (r = 0.999 8) g · L-1 respectively. The RSDs of precision were 3.19% and 1.17% , And the repeatability RSD was 1.40% and 1.60% respectively. The average recoveries were 99.63% and 100.27% respectively. Pulsatilla total saponin 3 batches of Pulsatilla saponin B3 mass concentrations were 0.186,0.190,0.191 g · L-1, Pulsatilla BD, respectively 0.069,0.065,0.066 g · L-1. The cumulative release rates of Pulsatilla saponin B3 and Pulsatilla saponin BD in pH 7.4 phosphate buffer for 12 h were 91.30% and 74.97%, respectively. Conclusion: The established method is accurate and sensitive and suitable for the determination of the content and release of Pulsatilla indica emulsions.