中药复方有效成分群在陶瓷膜分离过程中的迁移研究

Migration study on ceramic membrane separation process of active ingredient population in compound Chinese materia medica

目的以复方板蓝根利咽颗粒(板蓝根、玄参、桔梗、甘草等)水提液为研究对象,探讨中药复方有效成分群在不同孔径陶瓷膜分离过程中的动态迁移规律,并比较其膜滤通量、固含物去除率。方法分别以200 nm和50 nm孔径陶瓷膜对复方板蓝根利咽颗粒水提液进行分离精制,连续多次取样,优化的HPLC法为Agilent Zorbox Eclipse XDB-C18色谱柱,乙腈-0.05%磷酸水溶液梯度洗脱,检测波长采用切换波长,体积流量1 m L/min,柱温30℃,进样量10μL,同时测定复方中腺苷、(R,S)-告依春、甘草苷、哈巴俄苷、桔梗皂苷D和甘草酸铵6种有效成分,考察其动态迁移率。结果 HPLC法可以同时测定复方中6种有效成分,对于复方板蓝根利咽颗粒水提液,在200 nm陶瓷膜分离过程中,6种有效成分的动态迁移率波动范围在71%~104%,平均迁移率85%,膜滤通量衰减较小,稳定通量在426~340 L/(m2·h),固含物去除率21.0%。在50 nm陶瓷膜中,6种有效成分的动态迁移率波动范围在83%~107%,平均迁移率83%,膜滤通量衰减较大,稳定通量在258~228 L/(m2·h),固含物去除率23.9%。结论初步探讨了中药复方有效成分群在2种不同孔径陶瓷膜分离过程的动态迁移情况,为现代陶瓷膜技术在中药精制中的推广应用奠定药效物质迁移理论基础。

Objective Taking the water extraction of Compound Banlangen Liyan Granules(Isatidis Radix,Scrophulariae Radix,Platycodi Radix,Glycyrrhizae Radix,etc.) as the research object to explore the dynamic migration regular of the active ingredient population of compound Chinese materia medica in different apertures in ceramic membrane separation process and compare its membrane filtration flux and solid inclusion removal rate.Methods The water extraction of Compound Banlangen Liyan Granules was separated with 200 nm and 50 nm aperture of ceramic membrane,respectively.Continuously sampling for many times was done in the ceramic membrane separation process.The optimized HPLC methods were as follows: chromatographic column was Agilent Zorbox Eclipse XDB-C18,mobile phase was acetonitrile-0.05% phosphoric acid in gradient elution at flow rate of 1 m L/min,detection wavelength was wavelength switching,injection volum was 10 μL,the column temperature was 30 ℃.The contents of six active ingredients [adenosine,(R,S)-goitrin,liquiritin,harpagosid,platycodin D,and monoammonium glycyrrhizinate] were determined in the compound at the same time,and the dynamic migration rates were investigated.Results The simultaneous determination of the six active ingredient in the compound was done with HPLC method.For the water extraction in Compound Banlangen Liyan Granules,in the 200 nm ceramic membrane separation process,the dynamic migration rates of the six active ingredients ranged between 71%—104%,the average migration rate was 85%,the membrane filter flux attenuation was smaller,the stable flux was in 426—340 L/(m2·h),solid inclusion removal rate was 21.0%.But in 50 nm ceramic membrane,the dynamic migration rates of the six active ingredients ranged between 83%—107%,the average migration rate was 83%,the membrane filter flux attenuation was larger,the stable flux was in 258—228 L/(m2·h),and solid inclusion removal rate was 23.9%.Conclusion The experiment preliminarily reflects the dynamic migration regular of the active ingredient population of compound Chinese materia medica in two different aperture ceramic membrane separation process.It lays a migration theoretical foundation of effective materials for popularization and application of modern ceramic membrane technology in Chinese materia medica refining.