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目的:建立板蓝根水提液中(R,S)-告依春的含量测定方法,优选板蓝根水提液的陶瓷膜微滤精制工艺。方法:采用HPLC测定(R,S)-告依春含量,流动相甲醇-水-磷酸-三乙胺(14.0∶85.3∶0.6∶0.1),检测波长245 nm。以板蓝根水提液中有效成分(R,S)-告依春转移率、除杂率为指标,采用单因素试验法优选陶瓷膜孔径并测定精制前、后板蓝根水提液的浊度。结果:(R,S)-告依春在0.002 5~0.248μg与峰面积成良好线性关系(r=0.999 9),平均加样回收率98.9%,RSD 1.9%。优选的精制工艺为陶瓷膜孔径200 nm,进口压力0.2 MPa,当储液桶中药液量无法循环时,加相当于膜滤系统最少循环量的水顶洗1次,当膜滤液量等于原液量时结束微滤,该陶瓷膜微滤液的(R,S)-告依春转移率(87.8±1.9)%,除杂率(18.7±0.4)%。200 nm膜滤液,50 nm膜滤液,10 nm膜滤液的浊度分别为(1.4±0.3),(1.5±0.2),(0.5±0.2)NTU,截留液的浊度依次为(181.0±2.1),(220.4±2.5),(226.2±2.4)NTU。结论:该方法快速、准确,精密度、稳定性、重复性均良好,可测定板蓝根水提液中(R,S)-告依春含量。3种孔径的陶瓷膜均能较好地分离板蓝根水提液体系中不溶性悬浮微粒物质,但各孔径间的澄清效果无差别。
Objective: To establish a method for the determination of (R, S) -derivatives in Radix isatidis, and optimize the microfiltration process of the aqueous solution of Radix Isatidis. Methods: The content of (R, S) -dehydic acid was determined by HPLC. The mobile phase was methanol-water-phosphoric acid-triethylamine (14.0:85.3:0.6:0.1). The detection wavelength was 245 nm. With the effective component (R, S) - in the extract of Radix isatidis, according to the rate of spring transfer and the removal rate of impurities, the pore size of the ceramic membrane was optimized by single factor test and the turbidity of the aqueous extract of Radix Isatidis was determined. Results: (R, S) - Evodia suzanne had a good linear relationship with the peak area (r = 0.999 9) at 0.002 5 ~ 0.248μg. The average recoveries were 98.9% and RSD 1.9%. The best purification process is ceramic membrane pore size of 200 nm, inlet pressure of 0.2 MPa, when the liquid in the tank can not be recycled, plus the equivalent of the membrane filtration system, the minimum cycle of water top wash 1 times, when the membrane filtrate is equal to the amount of liquid At the end of the micro-filtration, the (R, S) -delivery rate of the ceramic membrane microfiltration was 87.8 ± 1.9% and the removal rate was 18.7 ± 0.4%. The turbidity of 200 nm membrane filtrate, 50 nm membrane filtrate and 10 nm membrane filtrate were (1.4 ± 0.3), (1.5 ± 0.2) and (0.5 ± 0.2) NTU, respectively. Turbidity of retentate was (181.0 ± 2.1) , (220.4 ± 2.5), (226.2 ± 2.4) NTU. Conclusion: The method is rapid, accurate, accurate, stable and reproducible. The method can determine the content of (R, S) The three kinds of ceramic membranes with different pore sizes can separate insoluble suspended particulate matter in the aqueous extract of Radix Isatidis better, but there is no difference in the clarification effect between each pore.