衍生法结合液相色谱串联质谱法测定婴幼儿配方食品中维生素D  

Determination of vitamin D in infant formula food by derivatization combined with high-performance liquid chromatography-tandem mass spectrometry

作　　者：张美金 王岚 钟钰 官咏仪 金梦 林海丹 ZHANG Meijin;WANG Lan;ZHONG Yu;GUAN Yongyi;JIN Meng;LIN Haidan(Guangzhou Customs Technology Center,Guangdong Guangzhou 510623,China)

机构地区：[1]广州海关技术中心,广东广州510623

出　　处：《中国食品卫生杂志》2023年第9期1290-1296,共7页Chinese Journal of Food Hygiene

摘　　要：目的建立衍生法结合液相色谱串联质谱法测定婴幼儿配方食品中维生素D。方法试样经酶解、皂化、液-液萃取、4-苯基-1,2,4-三唑啉-3,5-二酮(PTAD)衍生化反应,经Atlantis?T3色谱柱分离,甲醇-5 mmol/L甲酸铵溶液作为流动相,梯度洗脱,采用电喷雾电离(ESI),正离子多反应监测模式(MRM)测定,同位素内标法定量。结果方法的线性关系良好,相关系数r>0.99,3个质量浓度水平的加标回收率为92.3%~94.2%,相对标准偏差为3.03%~5.34%(n=6),方法定量限为1μg/kg。结论该方法简便准确,灵敏度高,选择性强,适用于婴幼儿食品中维生素D的检测。Objective A method involving derivatization combined with liquid chromatography-tandem mass spectrometry was developed for the determination of vitamin D in infant formula food.Methods The samples were treated with enzymolysis,saponification,liquid-liquid extraction,and 4-phenyl-1,2,4-triazoline-3,5-dion derivatization.Chromatographic separation was performed using an Atlantis®T3 column,and gradient elution was performed using the methanol-5 mmol/L ammonium format solution as the mobile phase.The method applied positive electrospray ionization and multiple reaction monitoring mode and was quantified with the isotope internal standard method.Results A good linearity was obtained with a correlation coefficient above 0.99.The average recovery levels from three different ranged from 92.3%to 94.2%,and the relative standard deviations were between 3.03%and 5.34%(n=6).The limit of quantification was 1µg/kg.Conclusion This method is simple,accurate with high sensitivity and high selectivity,and suitable for the determination of vitamin D in infant formula food.

关 键 词：婴儿食品 液相色谱-串联质谱 维生素D 4-苯基-1 2 4-三唑啉-3 5-二酮 

分 类 号：R155[医药卫生—营养与食品卫生学]