Gas Chromatographic Studies of Vitamins D<sub>2</sub> and D<sub>3</sub>

Nair, Padmanabhan P.; Bucana, Corazon D.; deLeon, Stella; Da, Turner

doi:10.1021/ac60225a002

Cited by 64 publications

(17 citation statements)

References 14 publications

(12 reference statements)

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“…The iso-octane phase, which contained all of the unmetabolized vitamin D and the neutral fat, was concentrated, dissolved in ethanol and saponified with KOH in the presence of pyro-gall01 (Nair, Bucana, de Leon & Turner, 1965). Vitamin D was not destroyed by this procedure but any esters of the vitamin would be partly hydrolysed.…”

Section: )mentioning

confidence: 99%

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The Distribution and Storage of Vitamin D and its Metabolites in Human Tissues

et al. 1972

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S U M M A R Y1. The distribution of vitamin D and its metabolites in human tissues has been studied by the combined use of radioactive cholecalciferol and biological assays of antiricketic activity in tissue extracts.2. Injected radioactive cholecalciferol was cleared rapidly from the blood; unchanged vitamin D and various metabolites were detected subsequently in all tissues examined. The highest concentration of biological activity and radioactivity was in fat; this and, to a lesser extent, other tissues were shown to retain activity over a prolonged period of time.3. Adipose tissue and voluntary muscle are the principal sites of storage of vitamin D in man. Pre-existing tissue pools of vitamin D can, in some circumstances, invalidate the use of radioactively labelled cholecalciferol to trace the pattern of body distribution.4. Metabolically produced 25-hydroxycholecalciferol is also taken up from the blood into many tissues, probably by protein-binding. 5. Vitamin D is excreted in bile principally as more polar metabolites. Smaller amounts of cholecalciferol and 25-hydroxycholecalciferol are also excreted, and antiricketic activity has been demonstrated in the bile of individuals treated with vitamin D.6. An excess of cholecalciferol (or of 25-hydroxycholecalciferol) in the blood appears to be eliminated by the physicochemical processes of partition into tissue lipid and binding to tissue proteins. It is inferred tentatively that an increased concentration of vitamin D or of 25-hydroxycholecalciferol in the liver also causes an increased biliary excretion of these substances, and an increased hepatic formation and elimination of more polar metabolites of the vitamin.

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Section: )mentioning

confidence: 99%

“…Vitamin D was not destroyed by this procedure but any esters of the vitamin would be partly hydrolysed. The non-saponifiable material, including vitamin D, was extracted from the hydrolysis mixture into n-hexane (Nair et al, 1965). The hexane extract was combined with the stored methanolic extract for silicic acid chromatography.…”

Section: )mentioning

confidence: 99%

The Distribution and Storage of Vitamin D and its Metabolites in Human Tissues

et al. 1972

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“…The triniethylsilyl derivatives of sugars was also subject to investigation (36,404,476), as were also the same derivat,ives of vit,amins D2 and DB (355) and myoinositol (411).…”

Section: Gas Chromatographymentioning

confidence: 99%

Biochemical Analysis

Hamilton¹

1966

Anal. Chem.

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review covers the two year period commencing January 1, 1964 through December 31,1965, following directly on the previous review of the same title (201) in Analytical Chemistry.Those papers which describe advances and improvements in methods and instrumentation as applied to determinations in the field of biochemistry are listed.Routine applications of standard methods are not reported. For these reasons, references to many excellent papers were omitted. Even with such an arbitrary selection, many papers of importance and interest had to be noted and as a consequence critical appraisal had to be virtually eliminated.COMMUNICATION AIDS, NEW JOURNALS, AND NEW BOOKS

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“…Vitamin D3 and its metabolites are currently determined by radioimmunoassay (RIA) [8,9] and competitive protein binding assay (CPBA) [ 10,11 ] after tedious and time-consuming pretreatments which involve liquid-liquid [12][13][14] and solid-liquid extractions [15][16][17][18] in both cases and either (LC [16][17][18][19][20][21] or GC [ 13,14,[22][23][24][25][26][27]) for the latter. Several methods based on derivatization reactions (dehydration [28][29][30], cycloaddition [12, 31M1], silanisation [13,14,23,35,38] and charge-transfer complex formation [42]) have been implemented pre-column for either LC or GC, and postcolumn for LC. Laser excitation as an enhancer offluorimetric detection has been widely used in clinical chemistry, mainly coupled with LC [43][44][45] and CE [46,47]; however, no application for quantitation of vitamin D3 metabolites has been reported so far.…”

Section: Introductionmentioning

confidence: 99%

Enhanced sensitivity by laser-induced fluorescence for the determination of calcitriol and other vitamin D3 metabolites in plasma

et al. 1999

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SummaryA sensitive method for the determination of hydroxymetabolites of vitamin D3, , particularly calcitriol (1,25-(OH)2-D3), in human plasma is reported. The method is based on the use of laser-induced fluorescence detection as an alternative to conventional fluorimetry in an integrated cleanup/preconcentration, HPLC separation and post-column derivatization system. The derivatization step is based on a dehydration reaction which takes place in secosteroid structures at high temperature in a strong-acid medium. A LOD of 0.01 pg mL -1 (SNR=3) was obtained for each analyte with a linear dynamic range over 4 order of magnitude with excellent regression coefficients (-> 0.9922) in all cases. The precision was studied at two concentration levels and the RSDs values (for n= 5) were acceptable (between 2.6 and 4.7 %). The method was also checked by applying it to human plasma spiked with the target analytes and excellent recoveries were obtained. This is the first time that these species have been determined at the sub-pg mU 1 level.

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Gas Chromatographic Studies of Vitamins D₂ and D₃

Cited by 64 publications

References 14 publications

The Distribution and Storage of Vitamin D and its Metabolites in Human Tissues

The Distribution and Storage of Vitamin D and its Metabolites in Human Tissues

Biochemical Analysis

Enhanced sensitivity by laser-induced fluorescence for the determination of calcitriol and other vitamin D3 metabolites in plasma

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Gas Chromatographic Studies of Vitamins D2 and D3

Cited by 64 publications

References 14 publications

The Distribution and Storage of Vitamin D and its Metabolites in Human Tissues

The Distribution and Storage of Vitamin D and its Metabolites in Human Tissues

Biochemical Analysis

Enhanced sensitivity by laser-induced fluorescence for the determination of calcitriol and other vitamin D3 metabolites in plasma

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Gas Chromatographic Studies of Vitamins D₂ and D₃