SPE-HPLC法检测苍耳子复方制剂中苍术苷的含量  

Determination of atractyloside in compound preparations containing Xanthii Fructus by SPE-HPLC

作　　者：刘鹏[1,2] 刘玉红[1] 刘云华[1] 黄志芳[1] 陈燕[1] 易进海[1] 

机构地区：[1]四川省中医药科学院,成都610041 [2]四川医科大学,泸州646000

出　　处：《药物分析杂志》2015年第12期2138-2142,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：国家重点基础研究发展计划(973)项目(2009CB522804);四川省科技厅基本科研业务专项(A-2014N-5)

摘　　要：目的:建立苍耳子复方制剂中毒性成分苍术苷的含量测定方法。方法:应用正、反相硅胶柱层析分离方法自制苍术苷对照品;复方样品经大孔树脂柱和固相萃取小柱前处理,再应用离子对色谱测定苍术苷的含量。采用Agilent Eclipse XDB-C18(250 mm×4.6 mm,5.0μm)色谱柱,以乙腈-0.15%磷酸二氢钠溶液(含0.12%四丁基氢氧化铵,磷酸调p H至3.5)(39∶61)为流动相,流速1.0 m L·min^(-1),柱温30℃,紫外检测波长203 nm。结果:苍术苷对照品经HPLC归一化法分析纯度大于98.0%;苍术苷进样量在0.10~2.59μg范围内线性关系良好(r=1.000),平均回收率为95.7%(RSD=1.2%,n=6)。测定不同产地、不同剂型样品5批,苍术苷含量分别为226.3、464.6、3 8 6.1、6 6.0、1 0 4 4.7μg·g^(-1)。结论:所建立的方法经方法学验证,可用于苍耳子复方制剂中毒性成分苍术苷的质量控制。Objective： To establish a method for determination of atractyloside,a toxic component,in compound preparations containing Xanthii Fructus. Methods： Atractyloside reference was isolated and purified by normal,reversed phase silica gel column chromatography. Macroporous resin and solid phase extraction were used for sample pre-treatment,the atractyloside was detected with ion-pair chromatography. The chromatographic separation was carried out with an Agilent Eclipse XDB-C18column（ 250 mm × 4. 6 mm,5. 0 μm）; the mobile phase was composed of acetonitrile-0. 12% tetrabutylammonium hydroxide in 0. 15% sodium dihydrogen phosphate solution（ p H 3. 5 adjusted with phosphoric acid） at the proportin of 39∶ 61,the flow rate of 1. 0 m L·min^（-1）,the column temperature was 30 ℃,and the detection wavelength was 203 nm. Results： The purity of atractyloside reference substance was detected by HPLC,which was over 98. 0%. Atractyloside had good linear relationship in the range of0. 10-2. 59 μg and the correlation coefficient was 1. 000,and the average recovery was 95. 7% with the RSD being1. 2%（ n = 6）; the content results of 5 samples from different origins and varies of formulations were 226. 3,464. 6,386. 1,66. 0 and 1 044. 7 μg·g^（-1）. Conclusion： According to methodology validation,the developed method can be used for quality control of compound preparations containing Xanthii Fructus.

关 键 词：苍耳子 毒性成分 苍术苷 对照品 标准物质 离子对色谱法 

分 类 号：R917[医药卫生—药物分析学]