HPLC法测定清热通淋片中苦参碱和氧化苦参碱含量方法的建立及评价  

Establishment and evaluation of HPLC method to determine content of matrine and oxymatrine in Qingre Tonglin Tablet

作　　者：孙录[1] 史磊[2] 吕薇[1] 耿虹 王华[1] 

机构地区：[1]吉林大学中日联谊医院药剂科,吉林长春130033 [2]吉林大学第二医院药剂科,吉林长春130041 [3]吉林省食品药品检验所,吉林长春130033

出　　处：《吉林大学学报（医学版）》2012年第5期894-898,共5页Journal of Jilin University：Medicine Edition

基　　金：吉林省科技厅科技发展计划项目资助课题(200705288)

摘　　要：目的:建立高效液相色谱(HPLC)法测定清热通淋片中苦参碱和氧化苦参碱含量的新方法,优化清热通淋片质量的检测和控制。方法:采用HPLC法。以苦参碱、氧化苦参碱标准品为对照品,清热通淋片为样品。使用Agilent 1200高效液相色谱仪,色谱柱Genimi-C18(5μm,4.6mm×250mm),流动相为磷酸盐缓冲液(pH=3.0)-甲醇(93∶7),流速为0.8mL.min-1,柱温为35℃,检测波长为220nm,进样量为10μL。通过对HPLC法进行线性关系、专属性、稳定性、精密度、重复性和准确度试验以进行方法学考察。结果:苦参碱回归方程为Y=1 102.1X+15.423,其进样量在0.311 8～4.677 0μg范围内呈良好线性关系(r=0.999 9),平均加样回收率为97.1%,RSD=0.24%(n=6);氧化苦参碱回归方程为Y=1 106.6X+5.040 2,其进样量在0.029 8～0.446 4μg范围内呈线性关系(r=0.999 6),平均加样回收率为98.4%,RSD=1.52%(n=6)。在稳定性、精密度和重复性实验中,苦参碱和氧化苦参碱的RSD值分别为1.21%、1.47%;0.13%、2.76%;0.48%(苦参碱和氧化苦参碱之和的RSD)。结论:HPLC方法分离效果好、专属性强、简便、灵敏和准确,可作为清热通淋片中苦参碱和氧化苦参碱含量的测定方法。Objective To establish a new method to determine the contents of matrine and oxymatrine in Qingre Tonglin Tablet by high performance liquid chromatography（HPLC）,in order to optimize the quality evaluation and control of Qingre Tonglin Tablet.Methods HPLC method was adopted.Matrine and oxymatrine standards were the control substances and Qingre Tonglin Tablets were the experiment samples.Using Agilent 1200 high performance liquid chromatograph,the determination was performed on Genimi-C18（5 μm,4.6 mm×250 mm） column with mobile phase consisting of phosphate buffer solution（PH3.0）-methanol（93∶7） at the flow rate of 0.8 mL·min-1.The column temperature was 35℃.The detection wavelength was 220 nm and the injection volume was 10 μL.For the methodological study,the linearity,specificity,stability,precision and repeatability and accuracy of the HPLC method were tested.Results The regression equation of matrine was Y=1102.1X＋15.423,showing good linearity（r=0.999 9） in the range of 0.311 8-4.677 0 μg.the average recovery rate was 97.1%（RSD = 0.24%,n=6）.The regression equation of oxymatrine was Y=1106.6X＋5.040 2,showing good linearity（r=0.999 6） in the range of 0.029 8-0.446 4 μg;the average recovery rate was 98.4%（RSD=1.52%,n=6）.In the tests of stability,precision and repeatability,the RSD of matrine and oxymatrine were respectively 1.21%,1.47%;0.13%,2.76%;0.48%（RSD of the sum of matrine and oxymatrine）.Conclusion HPLC method is simple,sensitive,reliable,specific and has satisfactory separation results,and it is competent for the quality control of Qingre Tonglin Tablet.

关 键 词：高效液相色谱法 清热通淋片 苦参碱 氧化苦参碱 

分 类 号：R927.2[医药卫生—药学] R284.1