RP-HPLC同时测定消风止痒颗粒中9种化学成分  

Simultaneous Determination of Nine Constituents in Xiaofeng Zhiyang Granules by RP-HPLC

作　　者：王月清 WANG Yue-qing(Pharmacy Department of Jiangbei Hospital District,Zhongda Hospital Affiliated to Southeast University,Nanjing 210048,China)

机构地区：[1]东南大学附属中大医院江北院区药剂科,江苏南京210048

出　　处：《食品与药品》2021年第4期356-362,共7页Food and Drug

摘　　要：目的建立反相高效液相色谱(RP-HPLC)同时测定消风止痒颗粒中梓醇、阿魏酸、毛蕊花糖苷、苍术素、升麻素苷、5-O-甲基维斯阿米醇苷、胡薄荷酮、甘草苷和甘草酸铵的方法。方法采用Waters XTERRA C_(18)色谱柱(250 mm×4.6 mm,5μm);乙腈-1.5 mmol/L KH_(2)PO4溶液(稀磷酸调pH 3.5)(25:75)为流动相,梯度洗脱,流速1.0 ml/min;柱温:35℃,进样量:10μl。结果梓醇、阿魏酸、毛蕊花糖苷、苍术素、升麻素苷、5-O-甲基维斯阿米醇苷、胡薄荷酮、甘草苷和甘草酸铵9种成分能达到很好分离;其线性范围分别为9.076~63.53μg/ml(r=0.9995),4.660~32.62μg/ml(r=0.9997),8.452~59.16μg/ml(r=0.9993),4.028~28.19μg/ml(r=0.9996),5.088~35.62μg/ml(r=0.9994),4.992~34.94μg/ml(r=0.9991),8.020~56.14μg/ml(r=0.9992),3.792~26.55μg/ml(r=0.9993),4.116~28.81μg/ml(r=0.9991),平均加样回收率分别为99.74%,99.21%,99.54%,99.03%,99.91%,98.99%,100.04%,98.79%,99.09%,RSD分别为0.55%,0.92%,0.69%,0.81%,1.13%,0.72%,1.14%,0.59%,0.68%(n=6)。8批次消风止痒颗粒中梓醇、阿魏酸、毛蕊花糖苷、苍术素、升麻素苷、5-O-甲基维斯阿米醇苷、胡薄荷酮、甘草苷和甘草酸铵质量浓度分别为0.4101~0.4159 mg/g,0.2409~0.2448 mg/g,0.3989~0.4015 mg/g,0.1571~0.1599 mg/g,0.2557~0.2582 mg/g,0.2511~0.2551 mg/g,0.3842~0.3866 mg/g,0.1001~0.1018 mg/g,0.1251~0.1276 mg/g。结论方法简便快速、回收率高、重现性好,可用于提升消风止痒颗粒的质量标准。Objective To establish an RP-HPLC method for the simultaneous determination of catalpol,ferulic acid,verbascoside,atractylodin,prim-O-glucosylcimifugin,5-O-methylvisammioside,p-menthone,liquiritin and ammonium glycyrrhizinate in Xiaofeng Zhiyang Granules.Methods The analysis was performed on a Waters XTERRA C_(18) column(250 mm×4.6 mm,5μm)using acetonitrile-1.5 mmol/L KH_(2)PO4(adjusting to pH 3.5 with phosphoric acid)(25:75)at the flow rate of 1.0 ml/min as mobile phase of gradient elution.The column temperature was set at 35℃and the injection volume was 10μl.Results The linear ranges of catalpol,ferulic acid,verbascoside,atractylodin,prim-O-glucosylcimifugin,5-O-methylvisammioside,p-menthone,liquiritin and ammonium glycyrrhizinate were 9.076-63.53μg/ml(r=0.9995),4.660-32.62μg/ml(r=0.9997),8.452-59.16μg/ml(r=0.9993),4.028-28.19μg/ml(r=0.9996),5.088-35.62μg/ml(r=0.9994),4.992-34.94μg/ml(r=0.9991),8.020-56.14μg/ml(r=0.9992),3.792-26.55μg/ml(r=0.9993)and 4.116-28.81μg/ml(r=0.9991).The average recoveries(n=6)were 99.74%(RSD=0.55%),99.21%(RSD=0.92%),99.54%(RSD=0.69%),99.03%(RSD=0.81%),99.91%(RSD=1.13%),98.99%(RSD=0.72%),100.04%(RSD=1.14%),98.79%(RSD=0.59%)and 99.09%(RSD=0.68%),respectively.The contents of nine batches of the catalpol,ferulic acid,verbascoside,atractylodin,prim-O-glucosylcimifugin,5-O-methylvisammioside,p-menthone,liquiritin and ammonium glycyrrhizinate were 0.4101-0.4159 mg/g,0.2409-0.2448 mg/g,0.3989-0.4015 mg/g,0.1571-0.1599 mg/g,0.2557-0.2582 mg/g,0.2511-0.2551 mg/g,0.3842-0.3866 mg/g,0.1001-0.1018 mg/g and 0.1251-0.1276 mg/g.Conclusion The method is simple,rapid,and of high recovery and good reproducibility.It can be used to improve the quality standard of Xiaofeng Zhiyang Granules.

关 键 词：消风止痒颗粒 反相高效液相色谱 化学成分 质量标准 

分 类 号：R917[医药卫生—药物分析学]