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A new method for synthesizing regiospecific 3-position vitamin D conjugates is described. Reaction of either 25-dihydroxyvitamin D2 or 25-dihydroxyvitamin D3 with p-nitrophenylchloroformate resulted in conversion to the respective 3-p-nitrophenylcarbonates. Reaction of the p-nitrophenylcarbonates with amines produced the 3-carbamates in good yield. Careful selection of commercially available amines and non-acidic conditions made this pathway amenable to the preparation of fluorescent, chemiluminescent, or biotinylated conjugates. This strategy offers a general method for the preparation of vitamin D conjugates. 相似文献
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Adamec J Jannasch A Huang J Hohman E Fleet JC Peacock M Ferruzzi MG Martin B Weaver CM 《Journal of separation science》2011,34(1):11-20
Simultaneous and accurate measurement of vitamin D and 25-hydroxyvitamin D in biological samples is a barrier limiting our ability to define "optimal" vitamin D status. Thus, our goal was to optimize conditions and evaluate an LC-MS method for simultaneous detection and quantification of vitamin D(2) , vitamin D(3) , 25-hydroxyvitamin D(2) and 25-hydroxyvitamin D(3) in serum. Extraction and separation of vitamin D forms were achieved using acetone liquid-liquid extraction and by a reversed phase C8 column, respectively. Detection was performed on a triple quadrupole tandem mass spectrometer (QQQ-MS/MS) equipped with atmospheric pressure photo ionization source. The LOQs for all analytes tested were 1 ng/mL for hydroxylated molecules and 2 ng/mL for the parent vitamin Ds. RSD at lower LOQ (2 ng/mL) and in medium (80 ng/mL) and high (200 ng/mL) quality control samples did not exceed 20 and 15% CV, respectively. Accuracy of the method for determination of hydroxylated molecules was also validated using National Institutes of Standards and Technology standard samples and found to be in the range of 90.9-111.2%. In summary, a sensitive and reproducible method is reported for simultaneous quantification of vitamin D(2) , vitamin D(3) , 25-hydroxyvitamin D(2) and 25-hydroxyvitamin D(3) molecules in biological samples. 相似文献
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Existence of vitamin D3 and 25-hydroxyvitamin D3 in rat lymph 总被引:1,自引:0,他引:1
T Okano S Masuda M Ishimine J Murai Y Yamamoto T Kobayashi 《Chemical & pharmaceutical bulletin》1983,31(9):3233-3241
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Higashi T Suzuki M Hanai J Inagaki S Min JZ Shimada K Toyo'oka T 《Journal of separation science》2011,34(7):725-732
Vitamin D deficiency in an infant is associated with a wide range of adverse health outcomes in later life. A method for the quantification of 25‐hydroxyvitamin D3 [25(OH)D3, the best‐established indicator of vitamin D status] in neonatal dried blood spots (DBSs) using LC/ESI‐MS/MS has been developed and validated. The method employed two steps of derivatization, a Diels–Alder reaction with 4‐phenyl‐1,2,4‐triazoline‐3,5‐dione followed by acetylation, to enhance the detectability of 25(OH)D3 in ESI‐MS/MS and to separate 25(OH)D3 from 3‐epi‐25‐hydroxyvitamin D3 [3‐epi‐25(OH)D3], a potent interfering metabolite. 25(OH)D3 was extracted from two DBS punches (3 mm in diameter, equivalent to 5.3 μL of whole blood), purified using an Oasis HLB® cartridge, and subjected to derivatization prior to analysis with LC/ESI‐MS/MS. 25‐Hydroxyvitamin D4 was used as the internal standard. This method was reproducible (intra‐ and inter‐assay RSDs, <6.9%) and accurate (analytical recovery, 95.2–102.7%), and the LOQ was 3.0 ng/mL. The developed method enabled specific quantification of 25(OH)D3 in neonatal DBSs and detection of vitamin D deficiency without interference from 3‐epi‐25(OH)D3. 相似文献
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《Tetrahedron letters》1987,28(39):4589-4590
A highly stereoselective synthesis of the side chain of 25-hydroxyvitamin D2 and 1α,25-dihydroxyvitamin D2 is described. 相似文献
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A method is described for the determination of 25-hydroxyvitamin D3 in human blood serum. The problems of sensitivity and selectivity encountered with previous techniques were avoided by the formation of a highly fluorescent Diels-Alder adduct following solid-phase extraction of the vitamin. After excess of reagent had been eliminated, quantification was achieved by high-performance liquid chromatography. The recovery of the vitamin from serum was 76.4 +/- 1.76%. The precision of the method was determined, and the relative standard deviations were 8.38% at a concentration of 47.0 x 10(-9) mol dm-3, 6.74% at a concentration of 99.8 x 10(-9) mol dm-3 and 3.79% at a concentration of 146.8 x 10(-9) mol dm-3. The detection limit for the adduct was 2.93 x 10(-14) mol injected, for a signal-to-noise ratio of 3:1, and serum concentrations of 0.25 x 10(-9) mol dm-3 could easily be quantified. No interference from endogenous or exogenous substances was observed. 相似文献
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J.K. Wichmann H.E. Paaren M.A. Fivizzani H.K. Schnoes H.F. DeLuca 《Tetrahedron letters》1980,21(49):4667-4670
All four possible C-23 and C-25 stereoisomers of the title compound have been synthesized. One of these isomers is identical to the natural product. 相似文献
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Takeo Taguchi Satoshi Mitsuhashi Akiko Yamanouchi Yoshiro Kobayashi Hiroshi Sai Nobuo Ikekawa 《Tetrahedron letters》1984,25(43):4933-4936
23,23-Difluoro-25-hydroxyvitamin D3 was synthesized from 6β-methoxy-3α,5-cyclo-23,24-dinor-5α-cholan-22-ol. 相似文献
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24,24-Difluoro-25-hydroxyvitamin D3 () has been prepared from commercially available lithocholic acid derivative to study the role of 24-hydroxylation in the metabolism of vitamin D3. 相似文献
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Stereoselective synthesis of (25S)-25-hydroxyvitamin D3 26,23-lactone () is described starting from C-22 steroidal aldehyde and (S)-citramalic acid. The spectral properties of the compound are almost identical with those of the natural product. 相似文献
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Sachiko Yamada Masami Shiraishi Masayuki Ohmori Hiroaki Takayama 《Tetrahedron letters》1984,25(31):3347-3350
25-Hydroxyvitamin D2 as synthesized conveniently and stereoselectively for the first time by utilizing Sharpless' chiral epoxidation and the subsequent regio- and stereoselective methylation with lithium dimethylcuprate to introduce the desired chirality at C(24) and the reductive elimination of the vicinal hydroxy sulfone to introduce stereoselectively the double bond at C(22) of the target molecule. 相似文献
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Yoshiro Kobayashi Takeo Taguchi Norio Kanuma Nobuo Ikekawa Jun-ichi Oshida 《Tetrahedron letters》1981,22(43):4309-4312
Two new fluorinated 25-hydroxyvitamin D3 analogs, 26,26,26-trifluoro- 25-hydroxy () and 27-nor-26,26,26-trifluoro-25-hydroxyvitamin D3 (), were prepared from 24-phenylsulfonyl 25,26,27-triorcholest-5-en-3β-yl tetrahydropyranyl ether (). 相似文献
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Nessvi S Johansson L Jopson J Stewart A Reeder A McKenzie R Scragg RK 《Photochemistry and photobiology》2011,87(5):1173-1178
The study aim was to determine the contribution of ethnicity, objectively measured skin color and skin reaction-to-sun exposure to variations in 25-hydroxyvitamin D(3) [25(OH)D(3) ]. A multiethnic sample (European, Maori, Pacific and Asian) of 503 adult volunteers aged 18-85 years, recruited from Auckland and Dunedin in New Zealand, answered a questionnaire on sun exposure and self-defined ethnicity. Skin color was measured using a spectrophotometer and the Individual Typology Angle (ITA) calculated. A blood sample was collected 4 weeks later to measure 25(OH)D(3). 25(OH)D(3) was associated with ethnicity, but not self-reported skin reaction-to-sun exposure. Amongst the ethnic groups, Asians had the lowest mean 25(OH)D level (37.0 nmol L(-1)) and Europeans with lighter colored skin had the highest (57.9 nmol L(-1)). An association also was seen between 25(OH)D(3) and skin color, with an increase of 2-3 nmol L(-1) per 10° increase in ITA value, indicating higher 25(OH)D(3) with lighter skin color; but much of this association disappeared after adjusting for ethnicity. In contrast, ethnicity remained associated with 25(OH)D(3) after adjusting for ITA skin color and skin reaction-to-sun exposure. These results indicate that self-defined ethnicity was a major determinant of variations in serum 25(OH)D(3), while objective measures of skin color explained relatively little additional variation. 相似文献
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Yoshiro Kobayashi Takeo Taguchi Tadafumi Terada Jun-ichi Oshida Masuo Morisaki Nobuo Ikekawa 《Tetrahedron letters》1979,20(22):2023-2026
From cholenic acid 24,24-difluoro-25-hydroxyvitamin D3 and 24ξ-fluoro-25-hydroxyvitamin D3 were prepared. 相似文献
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建立了一种高通量液相色谱-串联质谱技术检测干血点(DBS)样本中25-羟基维生素D2[25(OH)D2]和25-羟基维生素D3[25(OH)D3]的方法.以DBS为样本,以4-苯基-1,2,4-三唑啉-3,5-二酮(PTAD)为试剂进行分析物衍生化,所需样本量仅约相当于6μL全血当量的DBS样本;使用甲醇直接超声提取分析物,避开了通常情况下DBS样本前处理中的全血复溶和蛋白质沉淀等繁琐步骤;整个前处理过程使用自动化液体处理平台实现自动化操作和高检测通量;以25(OH)D2-D6和25(OH)D3-D3为同位素内标,消除基质效应的影响.前处理后的样本进行LC-MS/MS分析,使用C18柱进行分离,流动相为甲醇(含5 mmol/L甲酸铵)-水(含5 mmol/L甲酸铵)(75:25,V/V),洗脱时间为4 min,使用多反应监测模式(MRM)定量.结果表明:25(OH)D2和25(OH)D3的检出限为0.12 ng/mL(S/N=3),定量限为0.94 ng/mL(S/N=10).25(OH)D2和25(OH)D3在0.94~120.00 ng/mL范围内线性关系良好,日内相对标准偏差(RSD)分别为1.4%~8.6%和3.7%~15.5%,日间RSD分别为4.0%~5.3%和3.8%~14.9%,平均回收率分别为91.7%±7.9%~108.5%±6.5%和94.8%±6.8%~101.3%±2.9%.DBS样本在不同温度(-20℃,22℃,37℃)下储存不同时间(0,1,2,3,5,7,14天)后的稳定性实验显示样本总体RSD°15%.以25(OH)D参考物质NIST SRM 972a中的Level 3制备标准DBS样本,25(OH)D2和25(OH)D3的回收率分别为110.3%和103.0%. 相似文献
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