维生素K1的快速高通量光诱导化学发光分析  

Rapid and High-throughput Determination of Vitamin K1 by Photo-induced Chemiluminescence Detection

作　　者：李云云[1] 章竹君[2] 张琰图[1] 

机构地区：[1]延安大学化工学院,陕西延安716000 [2]陕西师范大学化学与化工学院,陕西西安710062

出　　处：《分析测试学报》2014年第9期1050-1055,共6页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(30872371);陕西省重点实验室项目(12JS119)

摘　　要：基于物质的光化学诱导效应，建立了维生素K1的快速高通量光诱导化学发光分析法。不发荧光的维生素K1（VKl）经紫外光照射（15W／254nm）后转变为具有很高荧光量子产率的光化产物，进而使用双（2，4，6．三氯苯基）草酸酯（TCPO）-过氧化氢（H2O2）-VKl光化产物这化一学发光体系，测定其化学发光强度。实验对光化条件和化学发光条件分别进行优化，同时研究了咪唑对光化产物结构及其相应的光化产物化学发光机理的影响。结果表明：在优化实验条件下，光诱导化学发光强度与VKl质量浓度在0.007～3.333μg·mL。范围内呈良好的线性关系，方法检出限（S/N=3）为2.2ng·mL-1，对0.1μg·mL-1VKl溶液进行11次平行测定，得相对标准偏差（RSD）为2.7％，10min内可完成96个样品的快速测定。用于维生素Kl注射液及人血清中VKl含量的测定，回收率为96.0％～104.0％。该法灵敏度高、选择性好、试剂用量少、自动化程度高，特别适于高通量、大批量样品的快速分析。A rapid and high-throughput analytical method was developed for the determination of vitamin K1 using photoinduced chemiluminescence（PICL） detection. This method is based on ultraviolet irradiation（254 nm/15 W） of vitamin K1 to produce a fluorescent product which could be determined by peroxideoxalate chemiluminescence system using chemiluminescence detector. Influence of imidazole on photochemical product structure and chemiluminescence mechanism were studied. Under the optimum cond.itions, a good linear relationship between chemiluminescence intensity and concentration of VK1 over the range of 0.007 - 3.333μg·mL- 1 was obtained. The detection limit （ SIN = 3 ） for vitamin K1 was 2.2 ng·mL-1 , and the relative standard deviation（c =0.1 μg · mL-1 , n = 11 ） was 2.7%. The method could be used to analyze 96 samples in 10 min, and was successfully applied in the determination of vitamin K1 in injection and human serum by standard addition calibration, with recoveries of 96.0% - 104.0% . The results showed that the PICL method was rapid, high-throughput, simple, sensitive and selective, and was especially suitable for the analysis of a large number of samples.

关 键 词：维生素K1 高通量 紫外光照 化学发光 人血清 

分 类 号：O657.3[理学—分析化学] Q568[理学—化学]