摘要
目的:建立一种快速,有效的方法测定砂生槐种子中生物碱的种类和含量。方法:用 TLC 快速分离定性总生物碱,并结合 HPLC 进行精确定量。TLC 采用 Merck Silica gel 60 F_(254)薄层层析板,氯仿-甲醇-浓氨水(5:0.6:0.1)为展开系统对总碱中主要成份进行定性分析;而后用 HPLC 法对其中苦参碱,氧化苦参碱和槐果碱的含量进行测定。色谱柱为 VP-ODS(5 μm,150 mm×4.6 mm)柱,流动相为乙腈(A),含0.035%三乙胺的0.02 mol·L^(-1)醋酸铵溶液(B)进行梯度洗脱,检测波长210nm,流速1.0 mL·min^(-1),进样量20 μL。结果:TLC 分析结果表明生物碱中含有苦参碱,氧化苦参碱,槐果碱,槐定碱和金雀花碱等。HPLC 测定时氧化苦参碱,苦参碱,槐果碱分别在3.0~97.0、2.5~80.0和1.6~50.7 mg·L^(-1)范围内呈线性相关,r 分别为0.9996,0.9999,0.9999。结论:沙生槐种子中含有苦参碱,氧化苦参碱,槐果碱,槐定碱和金雀花碱,其中氧化苫参碱,苦参碱,槐果碱含量约为21%,9%,0.9%,本文建立的方法能快速准确的测定沙生槐总碱中氧化苦参碱,苦参碱,槐果碱的含量。
Objective:To study the alkaloids composition of Sophora moorcrofiiana seed and develop a method of simultaneous determination of the main alkaloids. Method:TLC seemed to be the most convenient analytical technique for fast investigation and its precision was controlled by HPLC. TLC method using silica gel 60 F254 with chloroform methanol ammonia water(5: 0. 6: 0. 1 v/v/v) as mobile phase has been developed to separate and qualify the total alkaloid. Then these samples were further investigated through our established HPLC method. Analysis was performed on VP - ODS column(5 μm, 150 mm ×4. 6 mm) with acetonitrile (A) ,0. 02 mol · L^-1 ammonium acetate buffer with 0. 035% triethylamine(B) as mobile phase . Carry out gradient elution and alkaloids were determined at 210 nm. The flow rate was 1.0mlmin^-1. Result:This method has good linearity and correlation coefficient: oxymatrine was 3.0 -97.0 mg · L^-1, matrine was 2. 5 -80. 0mg · L^-1,sophocaripine was 1.6 -50 . 7mg · L^-1. Conclusion: There are many kinds of alkaloids in seed of sophora moorcrofiiana, such as matrine, oxymatrine, sophocarpine, sophoridine and laburnine. And oxymatrine,matrine,sophocarpine accounts for 21, 9 and 0.9 percent of total alkaloid respectively. Also, this method is simple, accurate and reproducible for determination total alkaloid of Sophora moorcrofiiana.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2008年第7期1071-1074,共4页
Chinese Journal of Pharmaceutical Analysis