RP-HPLC法测定埃索美拉唑钠的有关物质

RP-HPLC determination of related substances of esomeprazole sodium

目的:建立RP-HPLC法测定埃索美拉唑钠有关物质的方法。方法:采用Venusil XBP C18(L)色谱柱(250 mm×4.6mm,5μm),流动相采用乙腈-磷酸盐缓冲液(pH 7.6)-水梯度洗脱,流速为0.8 mL.min-1,柱温为30℃,检测波长为302nm。结果:在选定的色谱条件下,主成分能与各杂质之间分离良好,5-甲氧基-2-巯基苯并咪唑、奥美拉唑砜N-氧化物、奥美拉唑砜、埃索美拉唑钠及奥美拉唑硫醚浓度分别在3.99～29.94μg.mL-1(r=0.9998)、4.06～30.45μg.mL-1(r=0.9999)、2.46～18.42μg.mL-1(r=0.9998)、3.96～29.67μg.mL-1(r=0.9994)、4.08～31.32μg.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和RSD分别为99.5%、0.6%;99.1%、0.3%;99.0%、0.6%;99.2%、0.9%、99.0%、0.7%(n=9)。结论:本方法可用于检测埃索美拉唑钠产品质量。

Objective： To establish a RP-HPLC method for the determination of related substances of esomeprazole sodium.Methods： The determination was performed on a Venusil XBP C18（L）column（250 mm×4.6 mm,5 μm）,with a mobile phase consisting of a mixture of acetonitrile and phosphate buffer（pH 7.6）by gradient elution.The column temperature was set at 30 ℃ with a flow rate of 0.8 mL·min-1 and the detective wavelength was 302 nm.Results： Related substances were completely separated from the main constituent.The calibration curves for 5-methoxy-2-mercaptobenzimidazole,omeprazole sulfone N-oxide,omeprazole sulfone,esomeprazole sodium and omeprazole sulfide revealed good linearities over the ranges of 3.99-29.94 μg·mL^-1（r=0.9998）,4.06-30.45 μg·mL^-1（r=0.9999）,2.46-18.42 μg·mL^-1（r=0.9998）,3.96-29.67 μg·mL^-1（r=0.9994）,4.08-31.32 μg·mL^-1（r=0.9998）,respectively.The recoveries of the above compounds were 99.5% with RSD of 0.6%,99.1% with RSD of 0.3%,99.0% with RSD of 0.6%,99.2% with RSD of 0.9%,99.0% with RSD of 0.7%,respectively.Conclusion： The method can be used for testing the product quality of esomeprazole sodium.