离子色谱法测定淀粉中的顺丁烯二酸(酐)  

Determination of maleic acid( anhydride) in starch by ion chromatography

作　　者：林高明[1] 陈梅兰[2] 胡忠阳 刘慧 叶明立 

机构地区：[1]磐安县疾病预防控制中心,浙江金华322300 [2]浙江树人大学生物与环境工程学院,浙江杭州310015 [3]赛默飞世尔科技有限公司上海实验室,上海201203

出　　处：《中国卫生检验杂志》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)

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.

关 键 词：离子色谱 淀粉 顺丁烯二酸(酐) 

分 类 号：O657.75[理学—分析化学]