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  

Separation and Determination of Ephedrine Alkaloids and 2,3,5,6-Tetramethyl Pyrazine in Ephedra Herba by HPLC

作　　者：李红霞[1] 丁明玉[1] 吕琨[1] 郁鉴源[1] 

机构地区：[1]清华大学化学系,北京100084

出　　处：《色谱》2001年第2期161-163,共3页Chinese Journal of Chromatography

基　　金：清华大学基础研究基金资助项目

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(15 0mm×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 .0 2mol/LKH2 PO4 乙酸 三乙胺 (体积比为 4∶96∶0 .2∶0 .0 1)为流动相 ,在 2 10nm波长下检测 ;测定川芎嗪时 ,以甲醇 水 乙酸 (体积比为 35∶6 5∶0 .5 )为流动相 ,在 2 90nm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 .0 3mg/L ,0 .0 2mg/L ,0 .0 3mg/L。该法准确、灵敏、快速。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 C 18 column (Nova Pak  C 18 , 3.9 mm i.d.×150 mm) by using methanol 0.02 mol/L KH 2PO 4 acetic acid triethyl amine (4∶96∶0.2∶ 0.01, V/V ) as mobile phase for the ephedrine alkaloids analysis and methanol H\-2O 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%.

关 键 词：高效液相色谱法 麻黄碱 伪麻黄碱 去甲基麻黄碱 去甲基伪麻黄碱 川芎嗪 麻黄 中药分析 

分 类 号：R284.1[医药卫生—中药学]