板蓝根水提液的陶瓷膜精制工艺

Optimization of Ceramic Membrane Microfiltration Purification Technology for Decoction of Isatidis Radix

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0.0025 ～0.248 μg与峰面积成良好线性关系（r=0.9999）,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 determination of （R,S）-epigoitrin in decoction of Isatidis Radix and optimize ceramic membrane microfiltration purification technology for decoction of Isatidis Radix.Method：The content of （R,S）-epigoitrin was determined by HPLC,chromatographic conditions were as follows：mobile phase of methanol-water-phosphoric acid-triethylamine （14.0 ∶ 85.3 ∶ 0.6 ∶ 0.1）,detection wavelength 245 nm.Single factor tests were used to optimize ceramic membrane aperture according to indexes of transfer rate of （R,S）-epigoitrin and removal rate of impurity,then turbidity of decoction of Isatidis Radix before and after purified was determined.Result：Standard curves of （R,S）-epigoitrin was linear in the range of 0.002 5-0.248 μg with r =0.999 9,the average recovery was 98.9％ with RSD of 1.9％.Optimal purification technology was as following：ceramic membrane aperture 200 nm,inlet pressure was 0.2 MPa,When liquid volume in reservoir barrel was not enough to circulate,water with equal to the amount of the least circulation volume of membrane filtration system was added to the barrel once,and when filtration volume was equivalent to the original,microfiltration was ended; Under these conditions,transfer rate of （R,S）-epigoitrin was （87.8 ± 1.9） ％,removal rate of impurity was （18.7 ± 0.4） ％.Turbidity of membrane filtrate with 200,50,10 nm were （1.4±0.3）,（1.5 ±0.2）,（0.5 ±0.2） NTU,Turbidity ofretentate were （181.0±2.1）,（220.4±2.5）,（226.2 ± 2.4） NTU.Conclusion：This determination method was rapid,accurate and stable with fine repeatability,it could be adopted to determined the content of （R,S）-epigoitrin.Ceramic membrane with 3 kinds of aperture could be well separated insoluble suspended particulate matter in aqueous extract of Isatidis Radix,but clarify effect had no difference among each aperture.