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摘 要:用RP-HPLC分离测定了麻黄及其制剂中的麻黄类生物碱及川芎嗪。采用色谱柱Nova-Pak®C18(150mm×3.9mmi.d.),二极管阵列检测器(DAD)。测定麻黄类生物碱时,以甲醇-0.02mol/LKH2PO4-乙酸-三乙胺(体积比为4∶96∶0.2∶0.01)为流动相,在210nm波长下检测;测定川芎嗪时,以甲醇-水-乙酸(体积比为35∶65∶0.5)为流动相,在290nm波长下检测。分别测定了麻黄原药材、中成药(小儿清肺丸、鹭鸶咳丸)中麻黄碱、伪麻黄碱、去甲基麻黄碱、去甲基伪麻黄碱和川芎嗪的含量,检出限分别为0.4mg/L,0.1mg/L,0.03mg/L,0.02mg/L,0.03mg/L。该法准确、灵敏、快速。
Abstract:A
sensitive and reliable high performance liquid chromatographic
method(HPLC) has been developed for the first time for the simultaneous
determination of the active ingredients of ephedrine alkaloids and
2,3,5,6-tetramethyl pyrazine (TMP) in Ephedra herba crude drug and two
Chinese traditional medicines (Xiao-er qingfeiwan and Lu-si kewan).
The HPLC assay was
performed on a reversed phase C18 column (Nova-Pak®
C18, 3.9
mm i.d.×150 mm) by using methanol-0.02
mol/L KH2PO4-acetic acid-triethyl amine (4∶96∶0.2∶0.01,
V/V) as mobile phase for the ephedrine alkaloids analysis and methanol-H2O-acetic
acid (35∶65∶0.5,V/V)
as mobile phase for TMP analysis. Regression
equations revealed the linear relationships (correlation coefficients: 0.991-0.998)
between the peak area of each constituent (E, PE, NE, NPE, TMP) and its
concentration. The
detection limits for E, PE, NE, NPE and TMP were 0.4
mg/L, 0.1
mg/L, 0.03
mg/L, 0.02
mg/L and 0.03
mg/L, respectively, and the recoveries ranged between 92%-103%.
The contents of E, PE, NE,
NPE, TMP in Ephedra herba, traditional medicine Xiao-er qingfeiwan and
Lu-si kewan were determined respectively. The
relative standard deviations (RSD) of the contents ranged between 1.1%-3%. |
基金项目:清华大学基础研究基金资助项目 作者简介:李红霞(1971-),女,清华大学博士后。 作者单位:李红霞(清华大学化学系,北京 100084) 丁明玉(清华大学化学系,北京 100084) 吕琨(清华大学化学系,北京 100084) 郁鉴源(清华大学化学系,北京 100084) 参考文献: [1]HUANG Tai-kang. The handbook of common Chinese
medicine and pharmacology. Beijing:Chinese Medicine Science and
Technology Press,1994. 1 624-1 631黄泰康.
常用中药成分与药理手册. 北京:中国医药科技出版社,1994.
1 624-1 631 |
原载于《色谱》2001 Vol.19 No.2
P.161-163
http://periodical.wanfangdata.com.cn/periodical/sp/sp2001/0101/0101ml.htm