GC/MS测定淀粉制品中顺丁烯二酸  

Determination of maleic acid in starch products by GC /MS

作　　者：王立媛[1] 吴平谷[1] 张晶[1] 汤鋆[1] 赵永信[1] 沈向红[1] 

机构地区：[1]浙江省疾病预防控制中心,浙江杭州310051

出　　处：《中国卫生检验杂志》2014年第5期639-640,共2页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立了一种用于淀粉制品中顺丁烯二酸含量的气相色谱-质谱联用检测方法。方法采用乙醇提取样品，超声萃取，高速离心后吸取上层清液，上层清液用三氟化硼乙醚溶液乙酯化处理，冷却后用正己烷萃取，气质联用选择离子方式（GC—MS—SIM）检测样品提取物中的顺丁烯二酸。结果该方法在淀粉、贡丸、米线、QQ糖等几类淀粉制品中顺丁烯二酸的加标回收率在89％～99％之间，相对标准偏差（RSD）〈10％，按取样2．0g计算，最低检测限达到1．0mg／kg。结论方法净化效果好，检测灵敏度、准确度均满足检测要求，具有操作简单、干扰少、快速、准确可靠等特点，可作为淀粉制品中顺丁烯二酸含量检测的确证方法。为市场监管提供良好的基础数据。Objective To establish a method for determination of maleic acid in starch products by GC/MS. Methods The samples were uhrasonicly extracted with ethanol, then centrifuged at high speed to get the supernatant. The supernatant liquid was methylated with boron trifluoride diethyl etherate solution, after cooling, the analytes were extracted by n - hexane for detection of maleic acid using GC - MS - SIM. Results The recovery rates of maleic acid in several starch products, such as starch, pork ball, rice noodles and QQ candy, were 89% N 99% ,with RSD 〈 10%. Calculated on the sample amount of 2.0 ml, the lowest detection limit was 1.0 mg/kg. Conclusion The method has the advantages of easy operation, less interference, rapidity, accuracy and satisfying sensitivity, purification effect, so it could be used for determining maleic acid in starch products, and providing basic data for market supervision.

关 键 词：气相色谱-质谱联用 淀粉制品 顺丁烯二酸 

分 类 号：O657.63[理学—分析化学]