STABLE ISOTOPE-LABELED VITAMIN-D, METABOLITES AND CHEMICAL ANALOGS - SYNTHESIS AND USE IN MASS-SPECTROMETRIC STUDIES

被引:19
作者
COLDWELL, RD [1 ]
TRAFFORD, DJH [1 ]
VARLEY, MJ [1 ]
KIRK, DN [1 ]
MAKIN, HLJ [1 ]
机构
[1] UNIV LONDON LONDON HOSP,COLL MED,DEPT CHEM PATHOL,TURNER ST,LONDON E1 2AD,ENGLAND
关键词
STEROIDS; VITAMIN-D METABOLITES; DEUTERIUM LABELING; GAS CHROMATOGRAPHY; MASS SPECTROMETRY;
D O I
10.1016/0039-128X(90)90010-9
中图分类号
Q5 [生物化学]; Q7 [分子生物学];
学科分类号
071010 ; 081704 ;
摘要
Methods for the measurement of vitamin D and its metabolites using stable isotope-labeled internal standards and mass spectrometry are reviewed. The synthesis of both labeled and unlabeled standards is illustrated, and details of the synthesis of (26,26,27,27,27-H-2(5))-25,26-dihydroxyvitamin D3 and (28,28,28-H-2(3))-24,25-dihydroxyvitamin D2 are given. The use of in vitro biologic systems for the production of further metabolites of deuterated 25-hydroxyvitamin D3 is discussed. Use of deuterated 25-hydroxydihydrotachysterol 3 as a substrate in the isolated perfused rat kidney has provided valuable data for the assignment of structure to a number of metabolites of 25-hydroxydihydrotachysterol 3 formed in this system.
引用
收藏
页码:418 / 432
页数:15
相关论文
共 51 条
[1]  
Porteous, Coldwell, Trafford, Makin, Recent developments in the measurement of vitamin D and its metabolites in human body fluids, J Steroid Biochem, 28, pp. 785-801, (1987)
[2]  
Jongen, VanGinkel, van der Vijgh, Kuiper, Netelenbos, Lips, An international comparison of vitamin D metabolite measurements, Clin Chem, 30, pp. 399-403, (1984)
[3]  
MayerE, Schmidt-Gayk, Interlaboratory comparison of 25-hydroxyvitamin D determination, Clin Chem, 30, pp. 1199-1204, (1984)
[4]  
Lawson, Calam, Colinet, Certification of cortisol in two lyophilised serum samples, BCR no. 192 and 193, Report EUR 9661 EN, (1985)
[5]  
Coldwell, Porteous, Trafford, Makin, Gas chromatography-mass spectrometry and the measurement of vitamin D metabolites in human serum or plasma, Steroids, 49, pp. 155-196, (1987)
[6]  
Makin, Trafford, Measurement of vitamin D and its metabolites by gas chromatography-mass spectrometry, Vitamin D: Basic and Clinical Aspects, pp. 497-521, (1984)
[7]  
Seamark, Trafford, Makin, The estimation of vitamin D and some metabolites in human plasma by mass fragmentography, Clin Chim Acta, 106, pp. 51-62, (1980)
[8]  
Bjorkhem, Holmberg, Mass fragmentographic assay of 25-hydroxyvitamin D<sub>3</sub>, Methods Enzymol, 67, pp. 385-393, (1980)
[9]  
Bjorkhem, Holmberg, A novel specific assay of 25-hydroxyvitamin D<sub>3</sub>, Clinica Chimica Acta, 68, pp. 215-221, (1976)
[10]  
Bjorkhem, Holmberg, Kristiansen, Pedersen, Assay of 1,25-dihydroxyvitamin D<sub>3</sub> by isotope dilution-mass fragmentography, Clin Chem, 25, pp. 584-588, (1979)