4-甲基吡啶中有关物质的HPLC测定

Quantification of the Related Substances in 4-Methylpyridine by High Performance Liquid Chromatography

建立了高效液相色谱法快速测定4-甲基吡啶中有关物质的分析方法。色谱柱为十八烷基硅烷键合硅胶（长250mm，内径4．6mm，填料粒径5um），流动相为磷酸氢二钾-乙睛（80：20），流速1．0mL／min，柱温为宣温，检测波长255nm，进样量20uL。测定结粜表明4．甲基毗啶进样援与峰面秘呈良好的线性关系，线性范嘲为1．0-6．0μg／mL，R^2=O．9999，检出限为20．0ng／mL。4-甲基吡啶中有关物质2．甲基吡啶平均网收率为99．1％（n=9），RSD为1．76％：3-甲基吡啶平均刚收率为99．0％（n=9），RSD为1．66％。结果表明所建立方法简便、灵敏、准确可靠，专属性强，可用于4-甲基吡啶中有关物质的分析。

To establish a rapid determination of the related substances in 4-Methylpyridine samples by high performance liquid chromatography. The column was C18（250×4.6 mm, 5 pro）. The mobile phase was K2HPO4- acetonitrile （80： 20） and the flow rate was 1.0 mL/rain, and the colmnn temperature was maintained at room temperature. Absorbance of the eluent was monitored at 350 nm with the sample volume of 20 μL. The standard curve was linear in the 1.0-6.0 9g/mL（R^2=0.9999）, with the determination limit of 20.0 ng/mL. The related substances average recovery of 2-Methylpyridine was 99.1%（n=9）, RSD 为 1.76 % and 3-Methylpyridine was 99.0 %（n=9）, RSD 1.66 %. The proposed method was simple, sensitive and accurate and could be applied to the determination of the related substances in 4-Methylpyridine samples.