急支糖浆HPLC特征指纹图谱研究及多成分定量测定  

Fingerprint and multi-components quantitative determination for Jizhi Syrup by HPLC

作　　者：王春雷[1] 姜建伟[1] 侯桂兰[1] 

机构地区：[1]浙江省肿瘤医院,浙江杭州310022

出　　处：《中草药》2016年第23期4192-4197,共6页Chinese Traditional and Herbal Drugs

摘　　要：目的 建立急支糖浆的HPLC指纹图谱，并测定其主要成分的量，为急支糖浆的质量控制提供可靠方法。方法 采用Waters XTerra RP18色谱柱（250 mm×4.6 mm，5 μm），以0.8%冰醋酸水溶液（含有0.2%三乙胺）-乙腈为流动相进行梯度洗脱，体积流量1.0 mL/min，柱温35℃，检测波长为280 nm。采用《中药色谱指纹图谱相似度评价系统》（2012年版）建立急支糖浆HPLC指纹图谱并进行相似度分析；通过与阴性对照及混合对照品色谱峰进行比对，确定共有峰归属及成分指认；并对指认出的成分进行定量分析。结果 在特征图谱研究中，共确定17个共有峰，图谱中2、8号峰来源于鱼腥草，4、10号峰来源于金荞麦，7、12、15号峰来源于四季青，1、13号峰来源于麻黄，16、17号峰来源于枳壳，而3、6号峰为鱼腥草、金荞麦和四季青共有峰。同时利用相似度软件对10批急支糖浆指纹图谱进行分析，各批次样品相似度在0.98以上；通过比对特征峰保留时间，指认出6种主要成分，分别为原儿茶酸（3号峰）、原儿茶醛（6号峰）、阿魏酸（7号峰）、绿原酸（10号峰）、盐酸麻黄碱（13号峰）和柚皮苷（16号峰）；10批样品中原儿茶酸量在3.122 1~3.270 0 mg/mL，原儿茶醛量在5.108 6~5.224 9 mg/mL，阿魏酸量在8.893 2~9.120 8 mg/mL，绿原酸量在6.792 1~6.931 0 mg/mL，盐酸麻黄碱量在2.154 4~2.236 2 mg/mL，柚皮苷量在4.125 8~4.183 3 mg/mL。结论 所建立的急支糖浆HPLC指纹图谱和定量测定分析方法快速、准确、灵敏度高、专属性强，可以有效地评价该制剂的质量。Objective To establish an HPLC fingerprint method of Jizhi Syrup and determine the contents of its main components.Methods The Waters XTerra RP-18（250 mm×4.6 mm,5 μm） column was used with a mobile phase of 0.8% acetic acid （containning 0.2% triethylamine） and acetonitrile gradient elution,the flow rate was 1.0 mL/min,the column temperature was 35℃,and the detection wavelength was 280 nm.The Similarity Evaluation System for Chromatographic Fingerprint of TCM（2012 edition） was used to establish the fingerprint spectra and analyze the similarity degree.The common peaks were identified by reference compounds and negative controls,and the content was detected.Results The fingerprint chromatography included 17 mutual peaks.Peak 2 and peak 8 were from Houttuyniae Herba,peak 4 and peak 10 were from Fagopyri Dibotryis Rhizoma,peaks 7,12,and 15 were from Ilicis Chinensis Folium,peaks 1 and 13 were from Ephedrae Herba,peaks 16 and 17 were from Aurantii Fructus,and peaks 3 and 6 were from Houttuyniae Herba,Fagopyri Dibotryis Rhizoma,and Ilicis Chinensis Folium.The similarity among the batches was more than 0.98.Based on the retention time of master compounds,six components[protocatechuic acid （peak 3）,protocatechualdehyde （peak 6）,ferulic acid （peak 7）,chlorogenic acid （peak 10）,ephedrine hydrochloride （peak 13）,and naringin （peak 16）]were identified and quantified.The contents of protocatechuic acid,protocatechualdehyde,ferulic acid,chlorogenic acid,ephedrine hydrochloride,and naringin in 10 batches of Jizhi Syrup were 3.122 1-3.270 0,5.108 6-5.224 9,8.893 2-9.120 8,6.792 1-6.931 0,2.154 4-2.236 2,and 4.125 8-4.183 3 mg/mL,respectively.Conclusion The established method has high sensitivity,fast,precise and specificity,and can be used for the quality control of Jizhi Syrup.

关 键 词：急支糖浆 HPLC 指纹图谱 质量控制 原儿茶酸 原儿茶醛 阿魏酸 绿原酸 盐酸麻黄碱 柚皮苷 鱼腥草 金荞麦 麻黄 四季青 前胡 紫菀 枳壳 甘草 

分 类 号：R286.02[医药卫生—中药学]