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试验优化了样品处理及色谱条件,建立了使用高效液相色谱法检测淀粉及其制品中顺丁烯二酸的方法。以10%甲醇水溶液作为提取溶剂,超声波提取15 min,复杂样品需使用淀粉酶解处理。色谱条件为:色谱柱:Venusil MP C18柱(4.6 mm×250 mm,5μm);流动相:5%甲醇的水溶液(0.1%磷酸),调pH到3.0;柱温:30℃;进样量:10μL;流速:1.0 mL/min;检测波长:215 nm。方法定量限为2.0 mg/kg,线性范围:0.1μg/mL~5μg/mL,γ2=0.999 9,回收率为81.5%~104%,日内精密度1.3%~3.3%,日间精密度2.0%~4.3%。方法操作简便,定量准确,易于推广。
The experiment optimized the sample processing and chromatographic conditions, and established a method for the determination of maleic acid in starch and its products by using high performance liquid chromatography. 10% methanol aqueous solution as the extraction solvent, ultrasonic extraction 15 min, complex samples need to use amylase treatment. The chromatographic conditions were: column: Venusil MP C18 column (4.6 mm × 250 mm, 5 μm); mobile phase: 5% methanol in water (0.1% phosphoric acid) 10 μL; flow rate: 1.0 mL / min; detection wavelength: 215 nm. The limit of quantification was 2.0 mg / kg. The linear range was 0.1μg / mL ~ 5μg / mL, γ2 = 0.999 9, the recovery was 81.5% -104%, intraday precision was 1.3% -3.3% ~ 4.3%. The method is simple, accurate and easy to popularize.