HPLC测定格列美脲有关物质的改进  

Improvement of HPLC Determination Method for Related Substances in Glimepiride

作　　者：牛冲[1] 刘明洁[1] 凌霄[1] 张冬梅[1] 

机构地区：[1]山东省食品药品检验所,济南250101

出　　处：《中国现代应用药学》2013年第5期522-525,共4页Chinese Journal of Modern Applied Pharmacy

摘　　要：目的改进格列美脲有关物质检测的高效液相色谱法。方法采用AgilentZorbaxSB．C18色谱柱（250mm×4．6mm，5μm），以磷酸二氢钠溶液（取0．5g磷酸二氢钠，加水500mL溶解，用磷酸调pH至2．5）-乙腈（50：50）为流动相，流速1．0mL min-1，检测波长为228nm。结果溶剂对杂质检测无影响，格列美脲与已知杂质分离度良好，杂质1与杂质2的定量限均为10ng mL-1，杂质l在0．3042～2．028μg·mL-1，杂质2在0．3162～2．108gg·mL-1内呈良好线性关系（r分别为0．9995和0．9997），平均回收率分别为100％和99％，RSD为1．4％和1-3％。结论改进的方法消除了溶剂对杂质检测的干扰，可用于格列美脲中有关物质的检测。OBJECTIVE To improve the method for determining related substances in glimepiride by HPLC. METHODS The determination was performed on an Agilent Zorbax SB-C18 column（250 mm×4.6 mm, 5 μm）, and the mobile phase consisted of 500 mL sodium dihydrogen phosphate solution （dissolve 0.5 g of sodium dihydrogen phosphate in 500 mL of water and adjust to pH 2.5 with phosphoric acid） and 50 mL of acetonitrile at the flow rate 1.0 mUmin-1. The detection wavelenth was 228 nm. RESULTS The solvents had no effects on the impurity determination. An excellent separation was achieved. The LOQs of impurity 1 and 2 were both 10 ng.mL-1. The linearity were found in the rang of 0.304 2-2.028 μg mL-1 and 0.316 2-2.108 μg.mL-1 for impurity 1 and 2 respectively. The corresponding average recoveries were 100% with RSD 1.4% for impurity 1 and 99% with RSD 1.3% for impurity 2. CONCLUSION The improved method eliminated the solvent disturbance to impurity determination, and is suitable for the determination of impurities in glimepirede.

关 键 词：格列美脲 有关物质 杂质 高效液相色谱法 

分 类 号：R917.101[医药卫生—药物分析学]