摘要
目的:建立香薷的HPLC指纹图谱及其咖啡酸、迷迭香酸、木犀草素、芹菜素、黄芩素-7-甲醚、香荆芥酚、麝香草酚7个成分的HPLC含量测定方法。方法:采用Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5μm),流动相为0.1%甲酸水溶液(A)-乙腈(B),梯度洗脱(0~17 min,12%B→20%B;17~30 min,20%B→30%B;30~40 min,30%B→45%B;40~55 min,45%B→54%B),流速为1.0 mL·min^(-1),检测波长为280、330 nm,柱温为30℃,进样量为5μL。结果:建立了香薷HPLC指纹图谱,共确定了14个共有峰,并指认其中5个共有峰,分别为咖啡酸(5号峰)、迷迭香酸(10号峰)、黄芩素-7-甲醚(12号峰)、香荆芥酚(13号峰)、麝香草酚(14号峰),17批香薷样品的相似度均>0.910;对17批药材中指认的7个成分进行含量测定,其质量浓度分别在1.04~52.0μg·mL^(-1)(r=0.9993,n=5)、6.0~300.0μg·mL^(-1)(r=0.9995,n=5)、0.12~5.88μg·mL^(-1)(r=0.9994,n=5)、0.12~5.84μg·mL^(-1)(r=0.9998,n=5)、2.42~120.8μg·mL^(-1)(r=0.9998,n=5)、2.24~112.0μg·mL^(-1)(r=0.9995,n=5)、10.2~510.0μg·mL^(-1)(r=0.9995,n=5)范围内线性关系良好,平均回收率为104.3%~97.2%,RSD为0.18%~2.2%;17批样品中咖啡酸、迷迭香酸、木犀草素、芹菜素、黄芩素-7-甲醚、香荆芥酚、麝香草酚含量范围分别为0.442~1.028、1.222~9.727、0.017~0.093、0.016~0.070、0.279~1.013、0.0659~1.673、5.007~9.293 mg·g^(-1)。结论:该方法操作简便、可靠,重复性好,能同时测定7个成分的含量,为有效控制香薷质量提供了更加全面的依据。
Objective:To establish a fingerprint and a method for the determination of caffeic acid,rosmarinicacid,luteolin,apigenin,negletein,carvacrol and thymol in Moslae Herba using high performance liquid chromatography(HPLC).Methods:HPLC analysis was performed on an Eclipse XDB-C18column(250 mm×4.6 mm,5μm)with the gradient elution of 0.1%formic acid solution(A)and acetonitrile(B)(0-17 min,12%B→20%B;17-30 min,20%B→30%B;30-40 min,30%B→45%B;40-55 min,45%B→54%B).The flow rate was 1.0 mL·min^(-1),and the detection wavelengths were 280 nm and 330 nm.The column temperature was 30℃and the injection volume was 5μL.Results:HPLC fingerprint spectrum of Moslae Herba was established.A total of 14 common peaks in the fingerprint of Moslae Herba were assigned,and 5 components were identified as caffeic acid(peak No.5),rosmarinic acid(peak No.10),negletein(peak No.12),carvacrol(peak No.13)and thymol(peak No.14).The similarity of 17 batches of Moslae Herba samples were all over 0.910.The contents of the above seven components identified in 17 batches were determined,and their concentrations were in the linear ranges of 1.04-52.0μg·mL^(-1)(r=0.9993,n=),6.0-300.0μg·mL^(-1)(r=0.9995,n=5),0.12-5.88μg·mL^(-1)(r=0.9994,n=5),0.12-5.84μg·mL^(-1)(r=0.9998,n=5),2.42-120.8μg·mL^(-1)(r=0.9998,n=5),2.24-112.0μg·mL^(-1)(r=0.9995,n=5),10.2-510.0μg·mL^(-1)(r=0.9995,n=5),respectively.The average recoveries were 104.3%-97.2%with RSDs of 0.18%-2.2.%.The contents of caffeic acid,rosmarinic acid,luteolin,apigenin,5,6-dihydroxy-7-methory-flavone,carvacrol,and thymol in 17 batches of samples were 0.442-1.028,1.222-9.727,0.017-0.093,0.016-0.070,0.279-1.013,0.0659-1.673,5.007-9.293 mg·g^(-1),respectively.Conclusion:The proposed specific HPLC fingerprint spectrum and quantitation method of seven components of Moslae Herba is simple,stable and repeatable,which can provide a reference for quality evaluation of Moslae Herba.
作者
叶梦倩
吴孟华
马志国
曹晖
张英
YE Meng-qian;WU Meng-hua;MA Zhi-guo;CAO Hui;ZHANG Ying(Research Center for TCM of Lingnan(Southern China)Jinan University,Guangzhou 510632,China;National Engineering Research Center for Modernization of Traditional Chinese Medicine Lingnan Resources Branch,Guangzhou 510632,China;Guangdong Key Lab of Traditional Chinese Medicine Information Technology,Guangzhou 510632,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2023年第2期236-244,共9页
Chinese Journal of Pharmaceutical Analysis
基金
广东省中医药信息化重点实验室(2021B1212040007)。
