淀粉及其相关制品中马来酸测定方法的比较研究

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 C18柱（250 mm×215;4.6 mm,5 μm）;流动相：A相：0.1 mol＆#183;L-1磷酸溶液;B相：乙腈;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：1.0 m·min^-1;进样量：5 μl;紫外检测波长：210 nm.柱温：室温.结果：马来酸在2～200 μg·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2 μg·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剂均可用于测定.结论：该方法可以作为相关标准建立的参考.

Comparison Study on Maleic Acid Determination in Starch and Related Products

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.