柱前衍生化法评价注射用奥美拉唑钠中EDTA-2Na·2H_(2)O含量差异

Omeprazole sodium for injection by precolumn derivatization method

目的:评估市售不同企业生产的注射用奥美拉唑钠中二水合依地酸二钠(EDTA-2Na·2H_(2)O)含量差异。方法:采用Titank C18(250 mm×4.6 mm,5μm),以0.5%磷酸二氢铵(用磷酸调pH至3.0)为流动相A,乙腈为流动相B,梯度洗脱,检测波长为254 nm,建立快速测定注射用奥美拉唑钠中EDTA-2Na·2H_(2)O量的柱前衍生化方法。并测定市售5个生产厂家15个批次注射用奥美拉唑钠中EDTA-2Na·2H_(2)O含量。结果:EDTA-2Na·2H_(2)O在10~200μg/ml的范围内线性关系良好(r=0.9999),重复性、中间精密度均满足要求,平均回收率为100.47%,RSD为0.78%,检测限为1μg/ml,定量限为3μg/ml。市售各厂家(A、B、C、E)与原研厂家(D)EDTA-2Na·2H_(2)O含量均在1.4 mg/支左右。结论:本文所建立的方法可用于测定注射用奥美拉唑钠中EDTA-2Na·2H_(2)O含量,本试验所测定的5个厂家所生产的注射用奥美拉唑钠中EDTA-2Na·2H_(2)O含量无明显差异。

Objective:To evaluate the content difference of EDTA-2Na·2H_(2)O in omeprazole sodium for injection from different enterprises.Methods:Titank C18(250 mm×4.6 mm,5μm)chromatographic column was used for separation with gradient elution by using 0.5%ammonium dihydrogen phosphate(adjust pH to 3.0 with phosphoric acid)and acetonitrile as mobile phase.The detection wavelength was 254 nm.A precolumn derivatization method was established and applied for the content determination of EDTA-2Na·2H_(2)O in 15 batches of omeprazole sodium injection from 5 manufacturers.Results:The linear relationship of EDTA-2Na·2H_(2)O within the range of 10~200μg/ml was good(r=0.9999).The repeatability and intermediate precision meet the requirements.The average recovery was 100.47%(RSD was 0.78%).The limit of detection was 1μg/ml,and the limit of quantification was 3μg/ml.The content of EDTA-2Na·2H_(2)O in omeprazole sodium injection from the commercially available manufacturers(A,B,C,E)and original manufacturer(D)was about 1.4 mg/tube.Conclusion:The method established in this study can be used to determine the content of EDTA-2Na·2H_(2)O in omeprazole sodium for injection,and there is no significant difference for the content of EDTA-2Na·2H_(2)O in omeprazole sodium for injection produced by five manufacturers.