高效液相色谱法测定淀粉及淀粉制品中的顺丁烯二酸与顺丁烯二酸酐总含量

建立了基于高效液相色谱(HPLC)测定淀粉及其制品中顺丁烯二酸和顺丁烯二酸酐总含量的方法。通过优化得到最佳样品前处理条件为乙醇体积分数5%,超声时间10 min。色谱分离检测的最佳分析条件为:流动相:甲醇-1‰磷酸(2∶98),色谱柱:Plastisil ODS C18(250 mm×4.6 mm,5μm),检测波长214 nm,流速1.0 mL/min,柱温30℃。该方法对顺丁烯二酸的定量下限为5.0 mg/kg,线性范围为0.25～100 mg/L,相关系数为0.999 7,平均加标回收率为88%～89%,相对标准偏差(n=5)小于2%,能够满足实际检测需要。

Determination of Maleic Acid and Maleic Anhydride in Starch Products by High Performance Liquid Chromatography

A high performance liquid chromatographic(HPLC) method was established for the analysis of the total contents of maleic acid and maleic anhydride in starch products.A better extraction method was developed by using 5% ethanol as extraction solvent and ultrasonic extraction time of 10 min.The optimal chromatographic separation conditions were as the follows:separation column:Plastisil ODS C18 column(250 mm×4.6 mm,5 μm);mobile phase:methanol-1‰ phosphoric acid(2:98);detection wavelength:214 nm;flow rate:1.0 mL/min;column temperature:30 ℃.The limit of quantitation for formaleic acid was 5.0 mg/kg,and the linear range were in the range of 0.25-100 mg/L with a correlation coefficient of 0.999 7.The average spiked recoveries were between 88% and 89% with RSDs(n=5) less than 2%.The method could satisfy the requirement for the determination of the total contents of maleic acid and maleic anhydride in actual sample.