雀梅藤中大麦芽碱含量测定方法学考察  

Methodological Study on the Content Determination of Hordenin in Sageretia Thea

作　　者：普琼 陈丽元 吴晖[1] Pu Qiong;Chen Liyuan;Wu Hui(Department of Pharmacy,First Affiliated Hospital of Kunming Medical University,Kunming 650032.China)

机构地区：[1]昆明医科大学第一附属医院药剂科,昆明650032

出　　处：《中国药师》2022年第7期1263-1266,共4页China Pharmacist

基　　金：云南省科技计划项目重大科技专项(编号:2018ZF014)。

摘　　要：目的:建立雀梅藤中大麦芽碱含量测定方法学且优化其提取工艺。方法:HPLC法,色谱柱为JADE-PAK■KM-C_(18)(250 mm×4.6 mm,5μm),流动相为甲醇-0.02 mol·ml^(-1)磷酸二氢钾(10%磷酸调节pH至2)(10∶90),流速为1.0 ml·min^(-1),检测波长为220 nm,柱温为30℃,进样量为10μl。采用正交试验L_(9)(3^(4))对溶媒、溶剂量、氨水量及提取时间等因素进行考察,以大麦芽碱含量作为评价指标,优化其提取工艺并进行验证。结果:大麦芽碱在0.0250~0.9500 mg·ml^(-1)浓度范围内线性良好(r=0.9997),精密度、重复性较好(RSD<2%),平均回收率为100.8%(RSD=1.96%,n=6)。优化后雀梅藤大麦芽碱最佳提取工艺为100 ml氯仿、1.5 ml氨水、提取15 min,验证试验表明大麦芽碱的平均含量为1.1729 mg·g^(-1)(RSD=0.79%,n=3)。结论:所优化的提取工艺稳定可靠,所建方法学简便、准确、高效,可用于雀梅藤的质量控制。Objective:To establish a method for the determination of hordenine in Sageretia thea(Osbeck)and optimize its extraction process.Methods:An HPLC method was adopted.The detection was performed on a JADE-PAK■KM-C_(18) column(250 mm×4.6 mm,5μm).The mobile phase consisted of methanol-0.02 mol·ml^(-1) potassium dihydrogen phosphate(pH was adjusted to 2 by 10%phosphoric acid)(10∶90)at a flow rate of 1 ml·min^(-1),and the detection wavelength was 220 nm.The column temperature was set at 30℃,and the injection volume was 10μl.L_(9)(3^(4))Orthogonal test was used to investigate the factors including solvent type,solvent amount,amount of ammonia water and extraction time,and the content of hordenine was used as an index to evaluate,optimize and verify the extraction process.Results:The concentration of hordenine showed a good linear relationship within the range of 0.0250-0.9500 mg·ml(r=0.9997),and the precision and reproducibility were good(RSD<2%).The average recovery was 100.8%(RSD=1.96%,n=6).The optimal extraction process of hordenine was with 100 ml chloroform,1.5 ml ammonia water and extracting 15 min.The verification test showed that the average content of hordenine was 1.1729 mg·g^(-1)(RSD=0.79%,n=3).Conclusion:The optimized extraction process is stable and reliable.The established method is simple,accurate and efficient,which can be used for the quality control of Sageretia thea(Osbeck).

关 键 词：雀梅藤 大麦芽碱 含量测定 方法学 正交试验 

分 类 号：R927.2[医药卫生—药学]