液相色谱-大气压化学电离串联质谱法测定婴幼儿配方奶粉中的维生素D  

Determination of vitamin D in infant formula using liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry

作　　者：严丽娟[1] 李文斌 洪煜琛[1] 吴敏[1] 徐敦明[1] 林立毅[1] 顾春燕 

机构地区：[1]厦门出入境检验检疫局技术中心,福建厦门361026 [2]北京迪马科技有限公司,北京100029

出　　处：《色谱》2017年第4期427-431,共5页Chinese Journal of Chromatography

基　　金：福建省自然科学基金项目(2016J01071;2014J01057);长三角科技合作项目(15395810100;16395810100)~~

摘　　要：建立了婴幼儿配方奶粉中维生素D的液相色谱-大气压化学电离串联质谱(LC-APCI-MS/MS)分析方法。样品经正己烷和甲基叔丁基醚混合溶液提取,ProElut VDC固相萃取柱净化,Kinetex C_(18)色谱柱分离,采用大气压化学电离(APCI)源、正离子扫描和多反应监测(MRM)模式对维生素D_2和维生素D_3进行检测,内标法定量。结果表明维生素D_2和维生素D_3在5~5 000μg/L范围内均具有良好的线性关系,检出限为2μg/kg,定量限为5μg/kg。在5、10和100μg/kg添加水平下,维生素D_2和维生素D_3的回收率为85.2%~105.3%,相对标准偏差为4.7%~8.1%。该方法简便准确,灵敏度高,适用于婴幼儿奶粉中维生素D的测定。A method using liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (LC-APCI-MS/MS) was developed for the determination of vitamin D in infant formula. The milk powder sample was extracted with hexane and tert. butyl methyl ether followed by clean. up with ProElut VDC cartridge. The LC separation was performed on Kinetex C-18 column (100 mmx4. 6 mm, 2. 6 mu m) by a gradient elution using water and acetonitrile as the mobile phases with a flow rate of 1. 0 mL/min. Identification of vitamin D-2 and vitamin D-3 was achieved by APCI-MS/MS using multiple reaction monitoring (MRM). The quantification analysis was performed by internal standard method. The calibration curves showed a good linearity in the range of 5-5 000 mu g/L. The limits of detection (LODs) for vitamin D-2 and vitamin D-3 in the formula were 2 mu g/kg. The limits of quantification (LOQs) for vitamin D-2 and vitamin D-3 in the formula were 5 mu g/kg. The average recoveries of vitamin D from milk powder spiked at 5, 10 and 100 mu g/kg levels were between 85. 2% and 105. 3%, and the relative standard deviations were between 4. 7% and 8. 1%. The simple, accurate and sensitive method is suitable for the determination of vitamin D in infant formula.

关 键 词：液相色谱-大气压化学电离串联质谱 维生素D 婴幼儿配方奶粉 

分 类 号：O658[理学—分析化学]