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作 者:曹进[1] 黄湘鹭[1] 王静文[1] 张庆生[1] 丁宏[1]
机构地区:[1]中国食品药品检定研究院食品化妆品检定所,北京100050
出 处:《中国药师》2014年第1期22-25,共4页China Pharmacist
基 金:科技部国际合作课题(编号:2011DFA31440);国家科技支撑计划项目(编号:2012BAK08B02)
摘 要:目的:建立淀粉及相关制品中马来酸的测定方法。方法:采用高效液相色谱法,色谱柱为xBridge C_(18)柱(250 mm×4.6 mm,5μm);流动相:A相:0.1 mol·L^(-1)磷酸溶液;B相:乙晴;梯度:0/15 min,A相95%/10%;15~16 min,A相10%~0%;16~22 min,A相0%;22.1 min,A相95%;运行时间:30 min;流速:1.0ml·min^(-1);进样量:5μl;紫外检测波长:210 nm。柱温:室温。结果:马来酸在2~200μg·ml^(-1)的浓度范围有较好的线性.r=0.999 2,方法的检出限在不同产品中均为2μg·kg^(-1),平均回收率为85%~89%,RSD均小于5%。比较使用不同参照物质进行替代性检测情况,使用马来酸、马来酸氯苯那敏及其片荆均可用于测定。结论:该方法可以作为相关标准建立的参考。Objective: To establish a standard determination method for malelc acid in starch and its related products. Methods: The residue of maleic acid in starch and the related products was determined by HPLC. The column was an XBridge C18 (250 mm× 4.6 mm,μm) from Waters. The mobile phase A was 0.1 mol·L^-1 phosphoric acid, and the phase B was acetontrile. The gradient elution was with phase A 95%-10% in 0-15 min, 10%-0% in 15-16 min, 0% in 16-22 rain and 95% in 22.1 min. The total time was 30 min with a flow rate of 1.0 ml ·L^-1. The injection volume was 5 μl with the detection wavelength of 210nm at rnom temperature. Results : The optimized method for measuring maleic acid in starch and its related products was established with the linearity between 2 and 200 μg·ml^-1 ( r = 0. 999 2) , and the average limit of detection for different products was 2 μg·kg^-1 with RSD below 5 %. Alter- native reference substances, namely maleic acid, chlorpheniramine maleate and its tablets, were also compared with similar analysis results. Conclusion: The method can be used as the reference for the further standard establishment.
分 类 号:R917[医药卫生—药物分析学]
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