扶正辟邪合剂制备工艺及质量标准研究  

Preparation process and quality standard of Fuzheng Bixie Mixture

作　　者：罗群 蒲清荣 赵剑 黄锐 任桂林 唐定洪 李能源 杨思进 LUO Qun;PU Qingrong;ZHAO Jian;HUANG Rui;REN Guilin;TANG Dinghong;LI Nengyuan;YANG Sijin(Drug Manufacuturing Room,the Affiliated Traditional Chinese Medicine Hospital of Southwest Medical University,Sichuan Province,Luzhou646000,China;Department of Heart and Brain Diseases,the Affiliated Traditional Chinese Medicine Hospital of Southwest Medical University,Sichuan Province,Luzhou646000,China)

机构地区：[1]西南医科大学附属中医医院制剂室,四川泸州646000 [2]西南医科大学附属中医医院心脑病科,四川泸州646000

出　　处：《中国当代医药》2023年第10期7-11,共5页China Modern Medicine

基　　金：四川省中医药管理局科研应急攻关项目(2021X YCZ006);西南医科大学-西南医科大学附属中医医院联合项目(2020XYLH-004)。

摘　　要：目的优选扶正辟邪合剂的水提工艺,确定其质量标准。方法采用L9(34)正交试验法,以加水量、浸泡时间、煎煮时间、煎煮次数为影响因素,以绿原酸为指标,优选出扶正辟邪合剂的最佳煎煮工艺。采用薄层色谱法(TLC),以三氯甲烷-甲醇-水(13∶7∶2)下层溶液为展开剂,定性鉴别黄芪;以三氯甲烷-甲醇(8∶1)为展开剂,定性鉴别连翘。采用高效液相色谱法(HPLC)测定绿原酸的含量,色谱柱:Shim-pack VP-ODS(250 mm×4.6 mm,5μm),流动相:乙腈-0.4%磷酸溶液(13∶87),流速1.0 ml/min,柱温40℃,检测波长327 nm,进样量10μl。结果优选出扶正辟邪合剂的最佳煎煮工艺是:加8倍量水,浸泡0.5 h,提取3次,每次0.5 h。薄层色谱斑点显色清晰,阴性无干扰,专属性强。绿原酸在5.44~347.92μg/ml范围内与峰面积线性关系良好,线性方程为Y=27930X+9171.6(r^(2)=0.9999,n=7);精密度、稳定性、重复性良好,平均加样回收率为100.57%,RSD为0.97%(n=9)。测定3批扶正辟邪合剂样品中绿原酸的平均含量为0.30 mg/ml(RSD=1.9%)。结论该制备工艺简单可行,合理、有效,适用于扶正辟邪合剂的制备。建立的定性和定量质量控制方法操作简便,重复性好,可用于扶正辟邪合剂的质量控制。Objective To optimize the water extraction process of Fuzheng Bixie Mixture,and to study the quality standard.Methods L9(34)orthogonal test method was used with the mount of water added,soaking time,decoction duration and number of times of decoction as the influencing factors.The content of chlorogenic acid was taken as the evaluation indices to optimize the decoction process of Fuzheng Bixie Mixture.Thin layer chromatography(TLC)was used,and the lower solution of chloroform-methanol-water(13∶7∶2)was the developing agent to identify Astragail Radix.Chloroform-methanol(8∶1)was the developing agent to identify Forsythiae Fructus.The content of chlorogenic acid was determined by high performance liquid chromatography(HPLC).The column was Shim-pack VP-ODS(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.4%phosphoric acid solution(13∶87),the current speed was 1.0 ml/min,the column temperature was 40℃,the detection wavelength was 327 nm,and the sample volume was 10μl.Results The optimum water extraction process of Fuzheng Bixie Mixture was as follows:adding 8 times of water and soaking for 0.5 h,extracting 3 times,each time for 0.5 h.TLC spots were clear and well-separated without interference from negative sample.Chlorogenic was linear with peak area in the range of 5.44 to 347.92μg/ml and the linear equation was Y=27930X+9171.6(r^(2)=0.9999,n=7).The precision,stability,repeatability were good,and the average recovery was 100.57%with an RSD of 0.97%(n=9).The average content of Chlorogenic acid was 0.30 mg/ml(RSD=1.9%)among three batches of sample tablets.Conclusion The preparation process is simple,reasonable and effective,which is suitable for the preparation of Fuzheng Bixie mixture.The qualitative and quantitative quality control Methods established in the study shows simple and repeatable,which can be used for the quality control of Fuzheng Bixie Mixture.

关 键 词：扶正辟邪合剂 制备工艺 质量标准 绿原酸 

分 类 号：R283[医药卫生—中药学]