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.%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 - l%o 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.
展开▼
