摘要
目的建立高效离子色谱法测定淀粉中的顺丁烯二酸。方法样品加水混匀然后用离心机(3000 r/min)离心分离,取上清液过0.22μm滤膜后最过On-Guard RP小柱后进样分析。分离方法采用阴离子色谱柱IonPac AS22分离柱(250 mm×4 mm)和IonPac AG22保护柱(50 mm×4 mm),以4.5 mmol/L Na2CO31.4 mmol/L NaHCO3等度淋洗,进样量25μl,在流速1.0 ml/min的条件下,测定淀粉样品中顺丁烯二酸的含量。结果在0.05 mg/L^100 mg/L范围内线性关系良好,回归方程的线性相关系数为0.9999,在添加10 mg/kg、100 mg/kg、500 mg/kg 3个水平含量的马来酸,样品加标回收率在91%~95%之间,以信噪比(S/N)分别为3时和10时,检出限为0.83 mg/kg,定量限2.8 mg/kg。结论该方法具有灵敏度高,操作简单,重复性好等特点,能够快速准确测定淀粉中的顺丁烯二酸。
Objective To develop a new method for the determination of maleic acid （anhydride） in starch based on ion chro- matography. Methods Starch was dissolved in water, then centrifuged at 3000 r/min for 30 minutes. Then the solution was filtered through a 0.22 μm syringe membrane filter and On - Guard RP cleanup column for injection analysis. Mixture of 4.5 mmol/L sodium carbonate and 1.4 mmol/L sodium bicarbonate was selected as the elution, IonPac AS22（250 ×4 mm） as anion analytical column and IonPae AG22 as guard column（50 × 4 mm） were employed for separation. The sample injection volume was set at 25 μl for detection of maleic acid content by ion chromatography at the flow rate of 1.0 ml/min. Results The calibration curve of maleie acid was linear in the range of 0.05 mg/L ~ 100 mg/L（ r = 0.9999 ）. The recovery was between 91% -95% with maleie acid level at 10 mg/kg, 100 mg/kg and 500 mg/kg. When S/N was 3 and 10, the detection limit was 0.83 mg/kg, the quantitation limit was 2.8 mg/kg. Conclusion Ion chromatography method can accurately and quickly determine the content of maleie acid in starch with the advantages of high sensitivity, easy operation and good repeatability.
出处
《中国卫生检验杂志》
北大核心
2014年第5期668-669,673,共3页
Chinese Journal of Health Laboratory Technology
基金
国家自然科学基金(J0830413)
浙江省自然科学基金(Z14B070002)
