Li H X, Ding M Y, Lü K, Yu J Y
Department of Chemistry, Tsinghua University, Beijing 100084, China.
Se Pu. 2001 Mar;19(2):161-3.
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. x 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%.
首次建立了一种灵敏可靠的高效液相色谱法（HPLC），用于同时测定麻黄生药及两种中成药（小儿清肺丸和鹭鸶咳丸）中麻黄碱类生物碱和2,3,5,6 - 四甲基吡嗪（TMP）的活性成分。HPLC分析在反相C18柱（Nova - Pak C18，内径3.9 mm×150 mm）上进行，以甲醇 - 0.02 mol/L磷酸二氢钾 - 乙酸 - 三乙胺（4:96:0.2:0.01，V/V）为流动相分析麻黄碱类生物碱，以甲醇 - 水 - 乙酸（35:65:0.5，V/V）为流动相分析TMP。回归方程显示各成分（E、PE、NE、NPE、TMP）的峰面积与其浓度之间呈线性关系（相关系数：0.991 - 0.998）。E、PE、NE、NPE和TMP的检测限分别为0.4 mg/L、0.1 mg/L、0.03 mg/L、0.02 mg/L和0.03 mg/L，回收率在92% - 103%之间。分别测定了麻黄生药、中成药小儿清肺丸和鹭鸶咳丸中E、PE、NE、NPE、TMP的含量。含量的相对标准偏差（RSD）在1.1% - 3%之间。
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