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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2.0 g计算,最低检测限达到1.0 mg/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 the determination of maleic acid in starch products by gas chromatography-mass spectrometry. Methods The samples were extracted with ethanol and extracted by ultrasonic. The supernatant was extracted by high-speed centrifugation. The supernatant was ethyl esterified with boron trifluoride etherate, cooled and extracted with n-hexane. GC-MS- SIM) for the detection of maleic acid in the sample extract. Results The recoveries of maleic acid in starch, pork, rice noodle and QQ sugar were 89% -99%, relative standard deviation (RSD) <10% 2.0 g calculation, the minimum detection limit reached 1.0 mg / kg. Conclusion The method has good purification effect, detection sensitivity and accuracy to meet the test requirements. It has the characteristics of simple operation, less interference, quickness, accuracy and reliability. It can be used as the confirmation method for the determination of maleic acid in starch products. Provide good basic data for market supervision.