增强型基质去除净化-UPLC-Q-TOF/MS法快速测定奶粉中的香兰素类化合物

Rapid Determination of Vanillin Compounds in Milk Powder by EMR Purification Combined with UPLC-Q-TOF/MS

建立了超高效液相色谱-四极杆/飞行时间质谱法(Ultra performance liquid chromatography-quadrupole time of flight mass spectrometer,UPLC-Q-TOF/MS)对奶粉中的香兰素、甲基香兰素、乙基香兰素和香豆素的含量进行同时测定。样品以水溶解,乙腈提取后,盐析分层,离心后用增强型基质去除固相吸附剂(Enhanced matrix removal,EMR)净化上清液。在优化的仪器条件下,采用ESI和APCI复合源以正离子扫描方式进行采集。4种香兰素类化合物在2.0~200μg/L范围内呈良好线性关系,相关系数均大于0.9991。在6次平行测定中,平均回收率为77.0%~94.1%,相对标准偏差为2.76%~4.77%。方法检出限和定量限分别为10.0~20.0μg/kg和35.0~60.0μg/kg。该方法操作简便、条件简单,而且回收率好、灵敏度高、重现性好,可用于快速分析测定奶粉中4种香兰素类化合物的质量浓度。

An ultra performance liquid chromatography-quadrupole time of flight mass spectrometer(UPLC-Q-TOF/MS)method for rapid determination of four vanillin compounds including vanillin,methyl vanillin,ethyl vanillin and coumarin in milk powder was established.Samples were dissolved in water and extracted by acetonitrile.After salted out and centrifuged,the supernatant was purified by enhanced matrix removal(EMR).Under the optimized instrument conditions,data were collected with ESI and APCI composite sources by positive ion mode.All vanillin compounds exhibited good linearity within the concentrations of 2.0-200μg/L,while the coefficients of correlation were both greater than 0.9991.The average recoveries were ranged in 77.0%-94.1%with the relative standard deviations(RSDs)were2.76%-4.77%in six parallel examinations.The limits of detection and limits of quantitation were ranged in 10.0-20.0μg/kg and 35.0-60.0μg/kg respectively.This method was easy and simple conditions required to operate,in addition,good recovery,high sensitivity,high precision were possessed and it has practical value for rapid determination of four vanillin compounds in milk powder products.