那格列奈片的高效液相色谱分析

 目的：建立那格列奈片中主药那格列奈及杂质的高效液相色谱测定方法。方法：采用Shim-Pack CLC-ODSC 150 mmX 6.0 mm)色谱柱，曱醇-0.02 mol. L^-1磷酸盐缓冲液(pH 6.6)(75:25)作流动相,检测波长210 nm,含量测定采用外标法，杂质检查采用面积归一化法。考察了不同流动相下那格列奈的色谱行为及其与杂质的分离情况。结果：在优化的色谱条件下，片剂辅料不干扰测定，有关杂质与主药那格列奈分离良好，那格列奈线性范围5.1?101.0 mg·L^-1，最低检测限0.2 mg·L^-1，含量测定的回收率99.4%?100.4%，RSD<1.7%。结论：此法简便，准确，专属性强，重现性好，可用于那格列奈片的质量控制、稳定性考察和有效期预测。

Determination of nateglinide and impurities in nateglinide tablets by high performance liquid chromatography

OBJECTIVE To establish an HPLC method for determination of nateglinide and impurities in nateglinide tablets. METHODS Reversed-phase chromatographic separation was carried out on a Shim-Pack CLC-ODS column(150 mmX 6.0 mm) e-quilibrated with an eluent mixture constituted by CH₃OH-pH6.6, 0.02 mol·L^-1 phosphate buffer (7525). The detection was performed using ultraviolet detector at 210 nm. The effect of the type of mobile phase on separation of nateglinide and impurities in tablets was examined. The quantitative determination of nateglinide was performed with external standard method and the impurity limitation using area normalization method. RESULTS Nateglinide and impurities in tablets were separated completely under optimum conditions and no interference from excipients was found. Linear responses were observed for nateglinide concentration ranging from 5. 1 to 101.0 mg·L^-1 and the limit of quantification was 0.2 mg·L^-1. Assay precision expressed as RSD was less than 1.7% and the recoveries for nateglinide were in the range of 99.4% to 100.4% . CONCLUSIONS The proposed method is simple, accurate, reproducible, and highly selective. It is recommended that this method be used for the quality control, stability study and validity term test of nateglinide tablets.