某院自制制剂升清祛湿汤的质量评价方法研究  

Research on Quality Evaluation Method of Shengqing Qushi Decoction,a Hospital-made Preparation

作　　者：陈彤 万梅玲 贾先红 关承真 郭琳 CHEN Tong;WAN Mei-ling;JIA Xian-hong;GUAN Cheng-zhen;GUO Lin(Xuzhou City Hospital of TCM,Xuzhou Jiangsu 221000,China;The Affiliated Hospital of Xuzhou Medical University,Xuzhou Jiangsu 221000,China;Xuzhou Medical University School of Pharmacy,Xuzhou Jiangsu 221000,China)

机构地区：[1]徐州市中医院,江苏徐州221000 [2]徐州医科大学附属医院,江苏徐州221000 [3]徐州医科大学药学院,江苏徐州221000

出　　处：《抗感染药学》2023年第1期9-13,共5页Anti-infection Pharmacy

基　　金：江苏省药学会-天晴医院药学基金科研课题(编号:Q2019148)。

摘　　要：目的:建立医院自制制剂升清祛湿汤(Shengqing Qushi Decoction,SQD)的质量评价方法,为后续该制剂的质量评价提供参考。方法:以SQD为供试品,以葛根素、黄芪甲苷标准品为对照品,采用高效液相色谱法(HPLC)测定SQD中葛根素含量,采用高效液相色谱-串联质谱法(HPLC-MS/MS)测定SQD中黄芪甲苷含量,采用薄层色谱法(TLC)对SQD臣药组方黄芪、柴胡进行定性鉴别。结果:HPLC测定结果显示,葛根素的线性范围为4.88~43.92μg/mL,回归方程为ρ葛根素=42692 A-10100(r=0.9999);HPLC-MS/MS测定结果显示,黄芪甲苷的线性范围为28~6800 ng/mL,回归方程为ρ黄芪甲苷=6.31 A+12.60(r=0.9980);此外,葛根素和黄芪甲苷含量测定方法的精密度试验、重复性试验和加样回收试验均较为理想;SQD中葛根素和黄芪甲苷的平均含量分别为0.1523 mg/mL和1040.3333 ng/mL;TLC实验结果显示,SQD中黄芪和柴胡的性状斑点清晰。结论:采用HPLC和HPLC-MS/MS测定SQD中的葛根素和黄芪甲苷具有较好的准确度、精密度、重复性和稳定性,可较好地完成SQD的定量质量评价,而TLC法可对SQD中黄芪和柴胡进行较好地定性质量控制。Objective:To establish a quality evaluation method for Shengqing Qushi Decoction(SQD),a hospitalmade preparation,and provide a reference for subsequent quality evaluation of the preparation.Methods:By using SQD as the test sample,puerarin and astragaloside IV standards as the reference substances,the puerarin content in SQD was determined by high performance liquid chromatography(HPLC),the content of astragaloside IV in SQD was determined by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS),and the prescription of ministerial drug(astragalus,bupleurum)in SQD was qualitatively identified by thin-layer chromatography(TLC).Results:The determination results by HPLC showed that the linear range of puerarin was 4.88-43.92μg/mL,and the regression equation wasρ_(puerarin)=42692 A-10100(r=0.9999);the determination results by HPLC-MS/MS showed that the linear range of astragaloside IV was 28-6800 ng/mL,and the regression equation wasρ_(astragaloside)IV=6.31 A+12.60(r=0.9980);in addition,the precision test,repeatability test and spiked recovery test of the determination methods for the contents of puerarin and astragaloside IV were ideal;the average contents of puerarin and astragaloside IV in SQD were 0.1523 mg/mL and 1040.3333 ng/mL respectively;the TCL result showed that the spots of traits of astragalus and bupleurum in SQD were clear.Conclusion:The determination of puerarin and astragaloside IV in SQD by HPLC and HPLC-MS/MS has good accuracy,precision,repeatability and stability,which can be used to perform the quantitative quality evaluation of SQD,while the TLC method can be used to perform the qualitative quality control of astragalus and bupleurum in SQD.

关 键 词：升清祛湿汤 质量标准 葛根素 黄芪甲苷 高效液相色谱法 高效液相色谱-串联质谱法 薄层色谱法 

分 类 号：TQ460.72[医药卫生—药物分析学]