HPLC法同时测定壮药玉叶金花中9个成分的含量  

Simultaneous determination of nine components in Zhuang medicine Mussaenda pubescens Ait.f. by HPLC

作　　者：林雀跃 罗永强 张荣林 昝珂[3] 过立农[3] 谢培德 郑健[3] LIN Que-yue;LUO Yong-qiang;ZHANG Rong-lin;ZAN Ke;GUO Li-nong;XIE Pei-de;ZHENG jian(Guangxi Institute for Food and Drug Control, Nanning 530021, China;Guangxi-ASEAN Center for Food and Drug Safety Control, Nanning 530021, China;National Institutes for Food and Drug Control, Beijing 100050, China)

机构地区：[1]广西壮族自治区食品药品检验所,南宁530021 [2]广西-东盟食品药品安全检验检测中心,南宁530021 [3]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2018年第5期765-770,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：国家食药总局药化注册司专项"12种民族药材检验方法示范性研究";广西重大专项计划项目:壮药质量标准及质量控制技术规范化研究(桂科重1598005-10)

摘　　要：目的:建立HPLC法同时测定壮药玉叶金花中山栀苷甲酯、玉叶金花苷酸甲酯、8-O-乙酰山栀苷甲酯、新绿原酸、绿原酸、隐绿原酸、3,5-O-二咖啡酰基奎宁酸、3,4-O-二咖啡酰基奎宁酸及4,5-O-二咖啡酰基奎宁酸9个成分的含量。方法:采用CAPCELL MGⅡC_(18)色谱柱(4.6 mm×250 mm,5μm),以乙腈(A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱,流速1.0 mL·min^(-1),检测波长254 nm,柱温35℃,进样量10μL。结果:玉叶金花中9个成分在各自的线性范围内(新绿原酸0.151~189.2μg·mL^(-1),山栀苷甲酯0.768~960.4μg·mL^(-1),绿原酸0.775~968.7μg·mL^(-1),隐绿原酸0.886~1 107μg·mL^(-1),玉叶金花苷酸甲酯0.734~917.0μg·mL^(-1),8-O-乙酰山栀苷甲酯0.795~993.5μg·mL^(-1),3,4-O-二咖啡酰基奎宁酸0.872~1 090μg·mL^(-1),3,5-O-二咖啡酰基奎宁酸0.788~985.3μg·mL^(-1)和4,5-O-二咖啡酰基奎宁酸0.767~958.9μg·mL^(-1))均呈良好的线性关系,平均加样回收率、精密度、重现性和稳定性均符合有关规定。样品中9个成分的含量分别为新绿原酸0.30~1.57 mg·g^(-1),山栀苷甲酯0.34~5.20 mg·g^(-1),绿原酸0.34~5.84 mg·g^(-1),隐绿原酸0.32~2.26 mg·g^(-1),玉叶金花苷酸甲酯0.05~21.63 mg·g^(-1),8-O-乙酰山栀苷甲酯0.07~18.93 mg·g^(-1),3,4-O-二咖啡酰基奎宁酸1.02~4.21 mg·g^(-1),3,5-O-二咖啡酰基奎宁酸0.39~5.77 mg·g^(-1),4,5-O-二咖啡酰基奎宁酸1.38~5.25 mg·g^(-1)。结论:该方法可用于玉叶金花中9种成分的含量测定。Objective：To establish an HPLC method for the simultaneous determination of nine components,including shanzhiside methyl ester,mussaenoside,8-O-acetyl shanzhiside methyl ester,neochlorogenic acid,chlorogenic acid,cyrptochlorogenic acid,3,4-O-dicaffeoylquinic acid,3,5-O-dicaffeoylquinic acid and 4,5-O-dicaffeoylquinic acid,in Zhuang medicine Mussaenda pubescens Ait.f.Methods：HPLC analysis was performed on a CAPCELL MGⅡC（18） column（4.6 mm×250 mm,5μm）.The mobile phase was acetonitrile-0.1%phosphoric acid with gradient elution.The flow rate was 1.0 mL·min^（-1）,the detection wavelength was 254 nm,the column temperature was 35℃and the injection volume was 10μL.Results：The standard curve revealed a good linear relationship over the ranges of 0.151-189.2μg·mL^（-1） for neochlorogenic acid,0.768-960.4μg·mL^（-1） for shanzhiside methyl ester,0.775-968.7μg·mL^（-1） for chlorogenic acid,0.886-1107μg·mL^（-1） for cyrptochlorogenic acid,0.734-917.0μg·mL^（-1） for mussaenoside,0.795-993.5μg·mL^（-1） for 8-O-acetyl shanzhiside methyl ester,0.872-1090μg·mL^（-1） for 3,4-O-dicaffeoylquinic,0.788-985.3μg·mL^（-1） for 3,5-O-dicaffeoylquinic and0.767-958.9μg·mL^（-1） for 4,5-O-dicaffeoylquinic,respectively.Average recoveries,precision,reproducibility and stability were in accord with regulation.The contents of 9 components were 0.30-1.57 mg·g^（-1） for neochlorogenic acid,0.34-5.20 mg·g^（-1） for shanzhiside methyl ester,0.34-5.84 mg·g^（-1)for chlorogenic acid,0.32-2.26 mg·g^（-1） for cyrptochlorogenic acid,0.05-21.63 mg·g^（-1） for mussaenoside,0.07-18.93 mg·g^（-1） for 8-O-acetyl shanzhiside methyl ester,1.02-4.21 mg·g^（-1） for 3,4-O-dicaffeoylquinic,0.39-5.77 mg·g^（-1） for 3,5-O-dicaffeoylquinic and 1.38-5.25mg·g^（-1） for 4,5-O-dicaffeoylquinic,respectively.Conclusion：The developed method is suitable for the quantitative analysis of nine components in Mussaenda pubescens Ait.f.

关 键 词：玉叶金花 山栀苷甲酯 玉叶金花苷酸甲酯 乙酰山栀苷甲酯 新绿原酸 绿原酸 隐绿原酸 二咖啡酰基奎宁酸 天然药物 多组分测定 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]