同位素标记-超高效液相色谱-串联质谱法快速测定血清25-羟基维生素D3  

Rapid determination of serum 25-hydroxyvitamin D3 by isotope labeling-ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：郑仁锦[1] 华永有[1] 林守二 郑宓[2] 杨艳[1] ZHENG Renjin;HUA Yongyou;LIN Shouer;ZHENG Mi;YANG Yan(Fujian Provincial Center for Disease Prevention and Control/Fujian Provincial Key Laboratory of Zoonosis,Fuzhou,Fujian 350001,China;Second Affiliated People′s Hospital,Fujian University of Traditional Chinese Medicine,Fuzhou,Fujian 350001,China)

机构地区：[1]福建省疾病预防控制中心/福建省人兽共患病研究重点实验室,福州350001 [2]福建中医药大学附属第二人民医院,福建福州350001

出　　处：《现代医药卫生》2019年第16期2438-2440,共3页Journal of Modern Medicine & Health

基　　金：福建省卫生健康委员会青年科研课题资助项目(2017-1-26)

摘　　要：目的建立同位素标记-超高效液相色谱-串联质谱法快速测定血清25-羟基维生素D 3的方法。方法样品经乙腈提取,饱和硫酸锌沉淀蛋白,然后用正己烷萃取,氮气吹干后85%甲醇定容上样,以0.1%甲醇水-0.1%甲酸水为流动相,经ACQUITY BEH C 18(1.7μm,2.1 mm×100 mm)色谱柱分离,采用多重反应监测正离子模式进行检测。结果该方法在1~100 ng/L内线性关系良好;检出限0.3ng/kg;3个水平加标回收率为92.9%~98.9%,日内相对标准偏差为3.2%~4.2%,日间相对标准偏差为4.4%~4.9%。结论该方法操作简便、灵敏度高,适用于对血清25-羟基维生素D 3的快速检测。Objective To establish the method for rapidly determining serum 25-hydroxyvitamin D 3 by isotope labeling ultra performance liquid chromatography electrospray ionization tandem mass spectrometry(UPLC-ESI-MS/MS).Methods The samples were extracted with acetonitrile,the protein was precipitated by saturated zinc sulfate,then extracted with n-hexane,after drying with nitrogen,and sampled with 85%methanol at constant volume.The samples were separated by ACQUITY BEH C18(1.7μm,2.1 mm×100 mm)column using 0.1%methanol water-0.1%formic acid water as the mobile phase.The samples were detected by multiple reaction monitoring(MRM)positive ion mode.Results The method had a good linear relationship in the range of 1-100 ng/L,the detection limit(LOD)was 0.3 ng/kg,the recovery rates of three levels were 92.9%-98.9%,the intraday relative standard deviation(RSD)was 3.2%-4.2%and the interday RSD was 4.4%-4.9%.Conclusion This method is simple to operate,highly sensitive and suitable for rapid detection of serum 25-hydroxyvitamin D 3.

关 键 词：骨化二醇 血清 色谱法 高压液相 气相色谱-质谱法 同位素标记 维生素类 

分 类 号：R151[医药卫生—营养与食品卫生学]