HPLC-APCI(+)-MS/MS测定乳制品中的维生素D_2及D_3  

Determination of Vitamin D_2 and Vitamin D_3 in Dairy Products by HPLC- APCI( + )- MS/MS

作　　者：霍艳敏[1] 王骏 段文增[1,3] 薛霞 王艳丽 于文江 

机构地区：[1]聊城大学化学化工学院,山东聊城252000 [2]山东省食品药品检验研究院食品检验室,山东济南250101 [3]泰山学院化学化工学院,山东泰安271021

出　　处：《分析测试学报》2016年第3期327-331,共5页Journal of Instrumental Analysis

基　　金：山东省自然科学基金(ZR2012BL08)

摘　　要：建立了一种高效液相色谱-大气压化学电离串联四极杆质谱,正离子监测模式下（HPLC-APCI（＋）-MS/MS）测定乳制品中维生素D2和D3的方法。样品经皂化后,用石油醚提取,提取液经无水硫酸钠干燥,在氮气保护下旋转蒸发浓缩至10 mL以下,氮气吹干,用10 mL甲醇溶解后,经ACQUITY UPLC BEH C18色谱柱（1.7μm,2.1 mm×100 mm）分离,甲醇-水（95∶5）洗脱,多反应监测模式测定。维生素D2和D3在0.01-0.2 mg/L范围内呈良好的线性关系,相关系数（r2）分别为0.998 7和0.999 1,方法回收率为83.0%-99.4%,相对标准偏差（RSD）为2.0%-8.3%。An HPLC- APCI（ ＋）- MS- MS method was developed for the determination of vitamin D2（ VD2） and vitamin D3（ VD3） in dairy products. The sample was saponified,and then extracted with petroleum ether. Next,the extract was dried with anhydrous sodium sulfate and concentrated below 10 mL via rotary evaporation under the protection of nitrogen. Then it was dried with nitrogen and dissolved with 10 mL methanol. The extract was analyzed by HPLC- APCI（ ＋）- MS- MS using an ACQUITY UPLC BEH C18column（ 1. 7 μm,2. 1 mm × 100 mm） as chromatographic column with a mobile phase of methanol and water under gradient elution. The responses of VD2 and VD3showed good linearities in the range of 0. 01- 0. 2 mg / L,with correlation coefficients more than0. 998. The average recoveries were in the range of 83. 0%- 99. 4%, with RSDs of 2. 0%- 8. 3%.

关 键 词：高效液相色谱-串联四极杆质谱(HPLC-MS/MS) 大气压电离源 维生素D2 维生素D3 乳制品 

分 类 号：O657.63[理学—分析化学]