梯度洗脱RP-HPLC法测定吡贝地尔中的有关物质  

Gradient Eluting RP-HPLC Method for Determination of Related Substances in Piribedil

作　　者：李婷婷[1] 黄姗[1] 郑子栋[1] 

机构地区：[1]河南省食品药品检验所,郑州450003

出　　处：《中国药事》2014年第5期485-489,共5页Chinese Pharmaceutical Affairs

摘　　要：目的建立测定吡贝地尔中有关物质的RP-HPLC方法。方法采用RP-HPLC法，色谱柱为Supelcosil ABZ＋Plus（4．6mm×150mm，5μm），流动相为乙腈-水相，采用梯度洗脱，流速1．3mL·min^-1，柱温为40℃，检测波长240nm。结果在选定的色谱条件下，主成分与各杂质之间分离良好，2-哌嗪基嘧啶、胡椒醛、胡椒酸及吡贝地尔氧化产物浓度分别在3．83～13．40μg·mL^-1（r=0．9993）、4．83～16．90μg·mL^-1（r=0．9997）、3．01～10．55μg·mL^-1（r=0．9990）、3．22～11．26μg·mL^-1（r=0．9998）范围内与峰面积呈良好的线性关系。上述化合物的平均回收率依次为99．4％、101．1％、99．5％、100．3％；RSD依次为0．9％、0．8％、0．7％、0．7％（n=9）。结论本方法经方法学验证可用于检测吡贝地尔原料质量。Objective To establish an RP-HPLC method for determination of related substances in piribedil. Methods The determination was performed on a Supeleosil ABZ＋Plus （4.6 mm × 150 mm, 5 μm） column, with the mobile phase consisting of a mixture of acetonitrile and buffer by a gradient elution. The column temperature was set at 40 ℃ with a flow rate of 1.3 mL · min^-1 and the detection wavelength was 240 nm. Results Related substancesr peaks were completely separated from the main constituent peak. The calibration curves for products of 2-piperazinyl pyrimidine, piperonal, piperic acid and piribedil oxidation revealed good linearity over the range of 3.83-13.40 μg · mL^-1 （r=0. 9993）, 4. 83- 16.90 μg· mL^-1 （r=0. 9997）, 3.01-10.55 μg· mL^-1 （r=0. 9990）, 3.22-11.26 μg · mL^-1 （r=0.9998）. The recoveries of the four compounds were 99. 4%, 101.1%, 99.5%, 100. 3% , respectively. The RSDs were 0.9 %, 0.8%, 0.7%, and 0.7 % （n = 9）. Conclusion The methodology validation shows that the method can be used to detect the quality of the piribedil crude drug.

关 键 词：吡贝地尔 有关物质 2-哌嗪基嘧啶 胡椒醛 胡椒酸 吡贝地尔氧化产物 RP-HPLC 

分 类 号：R927.11[医药卫生—药学]