超高效液相色谱-四级杆-飞行时间质谱法定性检测胶类果仁膏中的胶类成分

Identification of gelatin ingredients in gelatin nut paste by ultra performance liquid chromatography quadrupole time of flight mass spectrometry

目的建立胶类果仁膏中的阿胶、黄明胶、新阿胶(猪皮胶)的专属性检测方法。方法采用胰蛋白酶对样品进行酶解,超高效液相色谱-四级杆-飞行时间质谱法(UPLC-Q-TOF)对果仁膏中的阿胶、黄明胶及新阿胶成分的专属性特征分子离子峰进行检测。结果阿胶选择质核比539.8(双电荷)→612.4和539.8(双电荷)→924.4的特征离子对;黄明胶选择质核比641.3(Z=2)→726.2和641.3(Z=2)→783.3的特征离子对;新阿胶选择质核比773.9(Z=2)→977.5和641.3(Z=2)→1 034.5的特征离子对时,均具有专属性。方法检出限:阿胶为10 mg/L、黄明胶为20 mg/L、新阿胶为5 mg/L。重复测定样品6次,显示方法稳定性良好。用该方法对10批实际样品(阿胶果仁膏)进行检测,仅2批检出阿胶。结论所建立的方法专属性强,可用于胶类果仁膏中阿胶、黄明胶及新阿胶的检测。

Objective To establish a method for the identificantion of donkey-hide gelatin,bovine-hide gelatin,pig-hide gelatin ingredients in gelatin nut paste.Methods The samples were digested with trypsin,and the ion peak of molecular characteristic of donkey-hide gelatin,bovine-hide gelatin,pig-hide gelatin was determined by ultra performance liquid chromatography quadrupole time of flight mass spectrometry（UPLC-Q-TOF）.Results The characteristic molecular peaks of donkey-hide gelatin were m/z 539.8（Z = 2） →612.4 and 539.8（Z = 2） →924.4; the ones of bovine-hide gelatin were m/z641.3（Z = 2） →726.2 and 641.3（Z = 2） →783.3,and the ones of pig-hide gelatin were m/z 773.9（Z = 2） →977.5 and641.3（Z = 2） →1034.5.All were specific.The detection limits of the method were as follows：donkey-hide gelatin was10 mg/L,bovine-hide gelatin was 20 mg/L,pig-hide gelatin was 5 mg/L.The established method was reliable after 6 times of repetative detections.The method was applied to 10 samples（donkey-hide gelatin nut paste）,donkey-hide gelatins were detected only in two samples.Conclusion The method is specific,and suitable for identification of donkey-hide gelatin,bovine-hide gelatin,pig-hide gelatin ingredients in gelatin nut paste.