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

J4 ›› 2012, Vol. 38 ›› Issue (5): 894-898.

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

孙录¹|史磊²|吕薇¹|耿虹³|王华¹

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

收稿日期:2012-06-13 出版日期:2012-09-28 发布日期:2012-09-28
通讯作者: 孙录（Tel：0431-84997594，E-mail：sunlugood@163.com） E-mail:sunlugood@163.com
作者简介:孙录（1958-）|男|吉林省榆树市人|副主任药师|主要从事医院药学研究。 
基金资助:
吉林省科技厅科技发展计划项目资助课题（200705288）

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

SUN Lu¹,SHI Lei²,LV Wei１,GENG Hong³,WANG Hua¹

1.Department of Pharmacy,China-Japan Union Hospital,Jilin University,Changchun 130033,China|2.Department of Pharmacy,Second Hospital,Jilin University,Changchun 130041, China|3. Jilin Institute for Food ＆ Drug Control,Changchun 130033,China

Received:2012-06-13 Online:2012-09-28 Published:2012-09-28

摘要/Abstract

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，4.6 mm×250 mm)，流动相为磷酸盐缓冲液（pH=3.0）-甲醇(93∶7)，流速为0.8mL/min，柱温为35℃，检测波长为220 nm，进样量为10 μL。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 0 μg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 4 μg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。

关键词: 高效液相色谱法；清热通淋片；苦参碱；氧化苦参碱

Abstract:

Abstract: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.The column temperature was 35℃.The detection wavelength was 220 nm and the injection volume was 10 μL.For the methodological study,thelinearity,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 issimple,sensitive, reliable,specific and has satisfactory separation results,and it is competent for the quality control of QingreTonglin Tablet.

Key words: high performance liquid chromatography, Qingre Tonglin Tablet, matrine, oxymatrine

中图分类号:

R927.2

孙录|史磊|吕薇|耿虹|王华. 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[J]. J4, 2012, 38(5): 894-898.

SUN Lu,SHI Lei,LV Wei,GENG Hong,WANG Hua. Establishment and evaluation of HPLC method to determine |content of matrine and oxymatrine in Qingre Tonglin Tablet[J]. J4, 2012, 38(5): 894-898.