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

摘要

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-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%．%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(150 mm×3．9 mm i.d.),二极管阵列检测器（DAD）。测定麻黄类生物碱时，以甲醇-0．02 mol/L KH2PO4-乙酸-三乙胺(体积比为4∶96∶0．2∶0．01)为流动相，在210 nm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290 nm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0．4 mg/L,0．1 mg/L,0．03 mg/L,0．02 mg/L,0．03 mg/L。该法准确、灵敏、快速。