摘要
目的:建立天仙子中消旋山莨菪碱、东莨菪碱和阿托品的含量测定方法及天仙子药材的HPLC特征图谱。方法:采用HPLC法对不同产地天仙子进行特征图谱研究,建立HPLC特征图谱共有模式,并进行相似度比较。色谱柱为资生堂CAPCELL-PAK C18(4.6 mm×250 mm,5μm),流动相为甲醇-乙腈-醋酸钠缓冲盐水溶液(5∶10∶85);流速1.0 ml/min;检测波长为210 nm;柱温:30℃。结果:消旋山莨菪碱、东莨菪碱及阿托品的线性范围分别为0.009 35~0.4676μg、0.054 63~2.7314μg和0.067 25~3.3623μg(r=0.9999);平均回收率分别为103.72%(RSD=1.72%)、98.57%(RSD=1.64%)和102.96%(RSD=1.26%);得到分离度较好的HPLC特征图谱,识别出5个特征共有峰。结论:本方法分离度较好,准确、可靠,为其质量控制提供了依据。
Objective: To develop an HPLC method for simultaneous determination of raceanisodamine, scopolamine and hyoscyamine in Henbane seeds and for study of specific chromatogram of Henbane seeds. Methods : The analysis was carried out on an Shiseido Capcell -Pak C18 (250 mm x 4.6 mm,5 μm) column;The mobile phase consisted of 0.1% phosphoric acid aqueous (A) and 70% acetonitrile (B) with gradient elution (0 - 30 min :60% A→35 % A ; 30 - 40 min : 35 % A→30% A ;40 - 44 min : 30% A→20% A;44-45 min:20% A→60% A;45 -60 min: 60% A)and the flow rate was 1.0 ml/min; the detection wavelength was 210 nm;the column temperature was 30 ℃. Result: The linear ranges of raceanisodamine, scopolamine and hyoscyamine were 0.009 35- 0.4676 μg ,0. 05463 - 2.7314 μg, and 0. 067 25 - 3. 3623 μg, respectively ( r 〉 0.9999 ) ; the average recoveries were 103.72% ,98.57% and 102.96%, respectively (RSD 〈 2% ,n = 6). Conclusion: This method is simple and can be used to determine the above three compents with satisfactory accuracy and repeatability.
出处
《天津药学》
2013年第2期4-7,共4页
Tianjin Pharmacy
关键词
高效液相色谱法
天仙子
消旋山莨菪碱
东莨菪碱
阿托品
特征图谱
HPLC, Henbane Seed, raceanisodamine, scopolamine, hyoscyamine, determination, specific chromatogram