高效液相色谱法测定蛋白粉中异麦芽酮糖含量  

Determination of isomaltulose content in protein powder by high performance liquid chromatography

作　　者：刘春丽 杨静 胡杰 卢迪勋 陈汉峰 黎俊威 LIU Chun-Li;YANG Jing;HU Jie;LU Di-Xun;CHEN Han-Feng;LI Jun-Wei(Access(Guangzhou)Testing Technology Service Co.,Ltd.,Guangzhou 510730,China)

机构地区：[1]捷通(广州)检测技术服务有限公司,广州510730

出　　处：《食品安全质量检测学报》2024年第24期71-76,共6页Journal of Food Safety and Quality

摘　　要：目的建立高效液相色谱法(high performance liquid chromatography,HPLC)测定蛋白粉中异麦芽酮糖含量。方法样品经50%乙腈超声萃取,离心后取上清液,经0.45μm微孔滤膜过滤后用亲水作用色谱(hydrophilic interaction liquid chromatography column,HILIC)分离,高效液相色谱仪-示差检测器分析。选用色谱柱Waters XBridge HILIC(4.6 mm×250 mm,5μm),流动相:乙腈:水=85:15(V:V);检测器温度为40℃;流速为1.0 mL/min;进样体积为5μL;柱温为40℃;运行时间为10 min。结果异麦芽酮糖在1.96~9.80 mg/mL范围内线性关系良好,相关系数(r^(2))为0.9999,回收率均大于90%(n=9),相对标准偏差为0.65%。本方法检出限为0.01 g/100 g,定量限为0.04 g/100 g。结论本方法前处理方法简单,检测灵敏度高,稳定性好,适用于蛋白粉样品中异麦芽酮糖含量的检测。样品使用50%乙腈水溶解样品能较好地除去部分杂质,同时采用Xbridge HILIC柱,有较好的极性保留,检测时间短,分离效果好,可以避免其他糖成分带来的干扰。Objective To establish a method for the determination of isomaltulose content in protein powder by high performance liquid chromatography(HPLC).Methods The sample was extracted by 50%acetonitrile ultrasonic extraction,centrifuged,and the supernatant was taken.It was filtered through a 0.45μm microporous membrane and separated by hydrophilic interaction liquid chromatography column(HILIC).The sample was analyzed by high-performance liquid chromatography differential detector.Select the Waters XBridge HILIC chromatographic column(4.6 mm×250 mm,5μm),mobile phase:Acetonitrile:water=85:15(V:V);the detector temperature was 40℃;the flow rate was 1.0 mL/min;the injection volume was 5μL;the column temperature was 40℃;the running time was 10 minutes.Results The linear relationship of isomaltulose was good within the range of 1.96–9.80 mg/mL,with a correlation coefficient of 0.9999 and recovery rates greater than 90%(n=9).The relative standard deviation value was 0.65%.The limit of detection of this method was 0.01 g/100 g,and the limit of quantification was 0.04 g/100 g.Conclusion This method has a simple pre-processing method,high detection sensitivity,and good stability,and is suitable for detecting the content of isomaltulose in protein powder samples.Dissolving the sample in 50%acetonitrile water can effectively remove some impurities,while using an Xbridge HILIC column has good polarity retention,short detection time,good separation effect,and can avoid interference from other sugar components.

关 键 词：高效液相色谱法 异麦芽酮糖 蛋白粉 亲水作用色谱 

分 类 号：O657.72[理学—分析化学] TS207.3[理学—化学]