骨骼风痛片的综合质量评价  

Comprehensive quality evaluation of Guge fengtong tablets

作　　者：吉顺莉[1] 周虹 王永智 殷晓芹[1] JI Shunli;ZHOU Hong;WANG Yongzhi;YIN Xiaoqin(Dept.of Pharmacy,the Affiliated Hospital of Nantong University,Jiangsu Nantong 226001,China;Dept.of Pharmacy,Hai’an People’s Hospital,Jiangsu Nantong 226600,China;School of Pharmacy,Nanjing University of Chinese Medicine,Nanjing 210023,China)

机构地区：[1]南通大学附属医院药学部,江苏南通226001 [2]海安市人民医院药剂科,江苏南通226600 [3]南京中医药大学药学院,南京210023

出　　处：《中国药房》2024年第8期948-954,共7页China Pharmacy

基　　金：江苏省高等学校基础科学(自然科学)研究重大项目(No.23KJA360007)。

摘　　要：目的建立测定骨骼风痛片中原薯蓣皂苷等11种成分含量的方法,同时进行化学计量学分析及熵权优劣解距离(EW-TOPSIS)法分析,以综合评价骨骼风痛片的质量。方法采用高效液相色谱法。以Agilent Eclipse Plus C18为色谱柱,以乙腈-0.2%磷酸溶液为流动相进行梯度洗脱,流速为1.0 mL/min,柱温为30℃,检测波长为203 nm(0~28 min,原薯蓣皂苷、甲基原薯蓣皂苷、伪原薯蓣皂苷、薯蓣皂苷)、280 nm(28~60 min,儿茶素、表儿茶素、甘草素、美迪紫檀素、6-姜辣素、8-姜酚、10-姜酚),进样量为10μL。以表儿茶素为内参物,采用一测多评(QAMS)法计算原薯蓣皂苷、甲基原薯蓣皂苷、伪原薯蓣皂苷、薯蓣皂苷、儿茶素、甘草素、美迪紫檀素、6-姜辣素、8-姜酚和10-姜酚的含量,并与外标法检测结果进行比较;采用SPSS 26.0、SIMCA14.1软件进行主成分分析和正交偏最小二乘法-判别分析,以变量重要性投影(VIP)值大于1为标准,筛选影响质量的差异标志物;采用EW-TOPSIS法对15批样品的质量进行综合评价。结果高效液相色谱结合QAMS法测得原薯蓣皂苷、甲基原薯蓣皂苷、伪原薯蓣皂苷、薯蓣皂苷、儿茶素、甘草素、美迪紫檀素、6-姜辣素、8-姜酚和10-姜酚的含量分别为6.330~10.863、1.150~2.274、0.431~0.740、2.818~4.823、0.826~1.510、0.043~0.094、0.079~0.231、0.479~1.020、0.146~0.288、0.118~0.318 mg/g,与外标法比较差异均无统计学意义(P>0.05);15批样品可分为3组,S1~S6、S7~S10、S11~S15分别聚为一组;原薯蓣皂苷、表儿茶素、薯蓣皂苷、6-姜辣素的VIP值均大于1;15批样品的最优解欧氏贴近度(Ci)为0.1635~0.7037,其中S11~S15样品的Ci值均大于0.6。结论所建QAMS法准确、简便,结合化学计量学分析及EW-TOPSIS法可用于综合评价骨骼风痛片的质量;原薯蓣皂苷、表儿茶素、薯蓣皂苷和6-姜辣素可能是影响骨骼风痛片质量的差异标志物;S11~S15样品的质量较好。OBJECTIVE To establish a method for the content determination of 11 components such as protodioscin in Guge fengtong tablets,and to evaluate the comprehensive quality of Guge fengtong tablets by combining with chemometric analysis and entropy weight-technique for order preference by similarity to ideal solution(EW-TOPSIS)method.METHODS HPLC method was adopted.The determination was performed on Agilent Eclipse Plus C18column with a mobile phase consisted of acetonitrile-0.2%phosphoric acid solution at the flow rate of 1.0 mL/min by gradient elution.The column temperature was set at 30℃.The detection wavelengths were set at 203 nm(0-28 min,protodioscin,methyl protodioscin,pseudoprotodioscin,dioscin)and 280 nm(28-60 min,catechin,epicatechin,liquiritigenin,medicarpin,6-gingerol,8-gingerol,10-gingerol);the sample size was 10μL.Using epicatechin as the internal reference,quantitative analysis of multi-components by single marker(QAMS)method was used to determine the contents of protodioscin,methyl protodioscin,pseudoprotodioscin,dioscin,catechin,liquiritigenin,medicarpin,6-gingerol,8-gingerol and 10-gingerol,which were compared with the results of the external standard method.SPSS 26.0 software and SIMCA 14.1 software were used for principal component analysis and orthogonal partial least squares-discriminant analysis,with variable importance in projection(VIP)value greater than 1 as the standard,to screen for differential markers that affect the quality;the EW-TOPSIS method was adopted to evaluate the quality of 15 batches of samples comprehensively.RESULTS The contents of protodioscin,methyl protodioscin,pseudoprotodioscin,dioscin,catechin,liquiritigenin,medi-carpin,6-gingerol,8-gingerol and 10-gingerol determined by HPLC combined with QAMS were 6.330-10.863,1.150-2.274,0.431-0.740,2.818-4.823,0.826-1.510,0.043-0.094,0.079-0.231,0.479-1.020,0.146-0.288,0.118-0.318 mg/g,respectively;there were no statistical significances,compared with the external standard method(P>0.05).A total of 15 batches of samples were clust

关 键 词：骨骼风痛片 一测多评法 化学计量学分析 熵权优劣解距离法 含量测定 差异标志物 

分 类 号：R917[医药卫生—药物分析学] R284[医药卫生—药学]