急支糖浆一板多药味HPTLC鉴别和HPLC含量测定方法的研究  

Study on HPTLC identification of one-plate multi-drug and HPLC content determination method for Jizhi syrup

作　　者：丁浩然 刘峰[1] 陈艳 王梦月[1] 李晓波[1] DING Haoran;LIU Feng;CHEN Yan;WANG Mengyue;LI Xiaobo(School of Pharmacy,Shanghai Jiaotong University,Shanghai 200240,China)

机构地区：[1]上海交通大学药学院,上海200240

出　　处：《中国药房》2022年第5期555-562,共8页China Pharmacy

基　　金：国家重点研发计划项目(No.2018YFC1707300)。

摘　　要：目的优化急支糖浆现有薄层色谱鉴别和含量测定方法。方法采用高效薄层色谱(HPTLC)法鉴别急支糖浆方中的四季青、鱼腥草、前胡、枳壳和甘草5种药材,采用高效液相色谱(HPLC)法测定原儿茶酸、盐酸麻黄碱和柚皮苷的含量。结果HPTLC法结果显示,具栖冬青苷、白花前胡甲素、柚皮苷、甘草苷4种对照品和鱼腥草对照药材的薄层斑点均显示清晰,比移值均在0.2~0.8范围内;经验证,方法专属性、耐用性和批次重复性良好。HPLC法结果显示,原儿茶酸、盐酸麻黄碱和柚皮苷的线性范围分别为4.32~431.67、1.14~114.17、7.02~702.33μg/mL(r均大于0.996);平均加样回收率分别为100.61%、100.40%、99.22%(RSD均小于2.00%);精密度(n=6)、稳定性(24 h,n=7)、重复性(n=6)试验的RSD均小于2.00%。原儿茶酸等3种活性成分在10批急支糖浆中的平均含量依次为623.3、152.1、1213.9μg/mL(RSD均小于10.00%)。结论本研究建立了急支糖浆一板多药味HPTLC鉴别方法,使用1种样品前处理方法、2个薄层色谱条件,实现了对处方中5种药材的快速鉴别;建立了HPLC含量测定方法,实现了对急支糖浆中3种活性成分的快速定量,可用于优化急支糖浆现有法定质量标准中的鉴别项和含量测定项。OBJECTIVE To optimize the existing thin layer chromatography(TLC)identification and content determination methods of Jizhi syrup.METHODS High performance thin-layer chromatography(HPTLC)was used to identify five medicinal materials in Jizhi syrup,such as Ilex chinensis,Houttuynia cordata,Peucedanum praeruptorum,Citrus aurantium,Glycyrrhiza uralensis.High performance liquid chromatography(HPLC)was used to determine the contents of procatechuic acid,ephedrine hydrochloride and naringin in Jizhi syrup.RESULTS HPTLC results showed that the identification spots of pedunculoside,praeruptorin A,naringin,and liquiritin were clearly displayed,and the retention factors were in the range of 0.2 to 0.8.After validation,the method had been proved to be strongly specific,robust and repeatable.HPLC results showed that the linear ranges of protocatechuic acid,ephedrine hydrochloride and naringin were 4.32-431.67,1.14-114.17 and 7.02-702.33μg/mL(all r>0.996),respectively.The average recoveries were 100.61%,100.40%and 99.22%,and RSDs were all less than 2.00%.RSDs of precision(n=6),stability(24 h,n=7)and repeatability(n=6)were all less than 2.00%.The average contents of the three components in 10 batches were 623.3,152.1,1213.9μg/mL(RSD<10.00%),respectively.CONCLUSIONS In this study,HPTLC method of one-plate multi-drug is established for the identification of Jizhi syrup.One sample pretreatment method and two TLC conditions are used to realize the rapid identification of five kinds of medicinal materials.An HPLC method is established to determine the content of Jizhi syrup,which realizes the fast quantification of three active components in Jizhi syrup,and can be used to optimize the identification and content determination items in the existing legal quality standards of Jizhi syrup.

关 键 词：急支糖浆 一板多药味 高效薄层色谱法 高效液相色谱法 含量测定 整体鉴别 

分 类 号：R286.0[医药卫生—中药学] R917[医药卫生—中医学]