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高效液相色谱法测定麻黄及其制剂中的麻黄类生物碱和川芎嗪

来源:中国色谱网
摘要: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。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......

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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, 39 mm i.d.×150 mm) by using methanol-002 mol/L KH2PO4-acetic acid-triethyl amine (49602001, V/V) as mobile phase for the ephedrine alkaloids analysis and methanol-H2O-acetic acid (356505,V/V) as mobile phase for TMP analysisRegression equations revealed the linear relationships (correlation coefficients: 0991-0998) between the peak area of each constituent (E, PE, NE, NPE, TMP) and its concentrationThe detection limits for E, PE, NE, NPE and TMP were 04 mg/L, 01 mg/L, 003 mg/L, 002 mg/L and 003 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 respectivelyThe relative standard deviations (RSD) of the contents ranged between 11%-3%
Keywordshigh performance liquid chromatography; ephedrine(E); norephedrine(NE); pseudoephedrine(PE); norpseudoephedrine(NPE); 2,3,5,6-tetramethyl pyrazine (TMP); Ephedra

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:

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原载于《色谱》2001 Vol.19 No.2 P.161-163
http://periodical.wanfangdata.com.cn/periodical/sp/sp2001/0101/0101ml.htm

 
作者: 李红霞 丁明玉 吕琨 郁鉴源 2007-5-18
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