Development and validation of a method for determination of plasma 25-hydroxyvitamin D3 3-sulfate using liquid chromatography/tandem mass spectrometry

Higashi, Tatsuya; Goto, Ayaka; Morohashi, Misato; Ogawa, Shoujiro; Kono, Kenji; Sugiura, T.; Fukuoka, Tomoki; Mitamura, Kuniko

doi:10.1016/j.jchromb.2014.08.027

Cited by 37 publications

(41 citation statements)

References 16 publications

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“…e plasma concentration of 25(OH) D 3 S was 30.1±12.2 ng/mL (mean±S.D., n=59) with the range of 3.9-65.1 ng/mL and signi cantly higher than that of 25(OH) D 3 (7.1±3.0 ng/mL, 2.7-17.0 ng/mL); these agreed with previously reported results. 5) As mentioned in the introduction, 25(OH) D 3 S might be the storage form of vitamin D 3 and utilized a er deconjugation to 25(OH) D 3 .…”

Section: Assay Precision and Accuracymentioning

confidence: 99%

“…25-Hydroxyvitamin D 3 3-sulfate [25(OH) D 3 S], the sulfated conjugate of 25(OH) D 3 , is another major metabolite of vitamin D 3 , and its circulating level was found to be much higher than that of 25(OH) D 3 in infants. 5) 25(OH) D 3 S might be the storage form of vitamin D 3 ; 25(OH) D 3 S may be utilized a er deconjugation to 25(OH) D 3 . [5][6][7] erefore, it is expected that the simultaneous determination of 25(OH) D 3 and 25(OH) D 3 S in plasma/serum is also helpful in the assessment of the vitamin D status and diagnosis for vitamin D de ciency/insufciency of newborns/infants.…”

Section: Introductionmentioning

confidence: 99%

“…5) 25(OH) D 3 S might be the storage form of vitamin D 3 ; 25(OH) D 3 S may be utilized a er deconjugation to 25(OH) D 3 . [5][6][7] erefore, it is expected that the simultaneous determination of 25(OH) D 3 and 25(OH) D 3 S in plasma/serum is also helpful in the assessment of the vitamin D status and diagnosis for vitamin D de ciency/insufciency of newborns/infants. Liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS) is now the most commonly used method to determine vitamin D metabolites in various biological samples due to its high speci city and accuracy.…”

Section: Introductionmentioning

confidence: 99%

“…5) Because 25(OH) D 3 S has a strong acidic and fragmentable moiety, i.e., a sulfate ester, it can be quanti ed without any derivatization. However, for the simultaneous quanti cation of 25(OH) D 3 and 25(OH) D 3 S, the DAPTADderivatization has the advantage of being able to remove the interference from 3-epi-25(OH) D 3 and provide the reliable measured values of 25(OH) D 3 .…”

Section: Introductionmentioning

confidence: 99%

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A Method for Simultaneous Determination of 25-Hydroxyvitamin D<sub>3</sub> and Its 3-Sulfate in Newborn Plasma by LC/ESI-MS/MS after Derivatization with a Proton-Affinitive Cookson-Type Reagent

et al. 2016

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A method for the simultaneous determination of 25-hydroxyvitamin D 3 [25(OH)D 3 ] and its 3-sulfate [25(OH)D 3 S] in newborn plasma, which is expected to be helpful in the assessment of the vitamin D status, using stable isotope-dilution liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS) has been developed and validated. e plasma was pretreated based on the deproteinization and solid-phase extraction, then subjected to derivatization with 4-(4-dimethylaminophenyl)-1,2,4-triazoline-3,5-dione (DAPTAD). e derivatization enabled the accurate quanti cation of 25(OH)D 3 without interference from 3-epi-25(OH)D 3 and also facilitated the simultaneous determination of the two metabolites by LC/positive ESI-MS/MS. Quanti cation was based on the selected reaction monitoring with the characteristic fragmentation of the DAPTAD-derivatives during MS/MS. is method was reproducible (intra-and inter-assay relative standard deviations of 7.8% or lower for both metabolites) and accurate (analytical recovery, 95.4-105.6%). e limits of quanti cation were 1.0 ng/mL and 2.5 ng/mL for 25(OH)D 3 and 25(OH)D 3 S, respectively, when using a 20-µL sample. e developed method was applied to the simultaneous determination of plasma 25(OH)D 3 and 25(OH)D 3 S in newborns; it was recognized that the plasma concentration of 25(OH)D 3 S is signi cantly higher than that of 25(OH)D 3 , and preterm newborns have lower plasma 25(OH)D 3 S concentrations than full-term newborns.

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Section: Assay Precision and Accuracymentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

A Method for Simultaneous Determination of 25-Hydroxyvitamin D<sub>3</sub> and Its 3-Sulfate in Newborn Plasma by LC/ESI-MS/MS after Derivatization with a Proton-Affinitive Cookson-Type Reagent

et al. 2016

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“…PTAD has been shown to exhibit limited stability (18 ); improved versions were reported by Higashi et al (17 ). The same group also described an isotope-coded differential analog of PTAD for relative quantification (19 ). Furthermore, a commercial derivatization reagent (Amplifex) is now available, which possesses a permanently charged quaternary ammonium group that substantially improves ionization efficiency (20 ).…”

Section: Limitations Of Lc-ms/ms Assaysmentioning

confidence: 99%

Mass Spectrometric Profiling of Vitamin D Metabolites beyond 25-Hydroxyvitamin D

Müller

Volmer

2015

Clinical Chemistry

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BACKGROUND:The frequency of measurements of vitamin D in the human population has significantly increased over the last decade because vitamin D has now been linked to many diseases, in addition to its established role in bone health. Usually, serum 25-hydroxyvitamin D concentrations are measured to assess the vitamin D status of individuals. Unfortunately, many studies investigating links between vitamin D and disease also use only this single metabolite. Intricate correlations with other vitamin D metabolites or dynamic effects of downstream metabolites may therefore be overlooked. Fortunately, powerful LC-MS/MS approaches have recently become available that can simultaneously quantify the concentrations of multiple vitamin D metabolites. These approaches are challenging, however, because of inherent instrumental problems with detection of vitamin D compounds and the low concentrations of the metabolites in biological fluids.CONTENT: This review summarizes recent mass spectrometry assays for the quantitative measurement of multiple vitamin D metabolites and their application in clinical research, with a particular focus on the lowabundance downstream metabolic species generated after the initial hydroxylation to 25-hydroxyvitamin D.

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Sulfation of vitamin D₃‐related compounds—identification and characterization of the responsible human cytosolic sulfotransferases

et al. 2017

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While 25-hydroxyvitamin D 3-O-sulfate is known to be present in circulation, how it is generated in the body remains unclear. This study aimed to investigate its sulfation in major human organs and to unveil the responsible cytosolic sulfotransferases (SULTs). Of the vitamin D -related compounds tested, 25-hydroxyvitamin D and 7-dehydrocholesterol are preferentially sulfated by human organ cytosols. Among the 13 human SULTs, SULT2A1 shows sulfating activity toward all vitamin D -related compounds, whereas SULT1A1 and SULT2B1a/SULT2B1b show sulfating activity exclusively for, respectively, calcitriol and 7-dehydrocholesterol. These findings suggest that the metabolic pathway leading to the formation of 25-hydroxyvitamin D 3-O-sulfate may be mediated by the sulfation of 25-hydroxyvitamin D or by the conversion of 7-dehydrocholesterol-3-O-sulfate in the skin.

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Development and validation of a method for determination of plasma 25-hydroxyvitamin D3 3-sulfate using liquid chromatography/tandem mass spectrometry

Cited by 37 publications

References 16 publications

A Method for Simultaneous Determination of 25-Hydroxyvitamin D<sub>3</sub> and Its 3-Sulfate in Newborn Plasma by LC/ESI-MS/MS after Derivatization with a Proton-Affinitive Cookson-Type Reagent

A Method for Simultaneous Determination of 25-Hydroxyvitamin D<sub>3</sub> and Its 3-Sulfate in Newborn Plasma by LC/ESI-MS/MS after Derivatization with a Proton-Affinitive Cookson-Type Reagent

Mass Spectrometric Profiling of Vitamin D Metabolites beyond 25-Hydroxyvitamin D

Sulfation of vitamin D₃‐related compounds—identification and characterization of the responsible human cytosolic sulfotransferases

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Development and validation of a method for determination of plasma 25-hydroxyvitamin D3 3-sulfate using liquid chromatography/tandem mass spectrometry

Cited by 37 publications

References 16 publications

A Method for Simultaneous Determination of 25-Hydroxyvitamin D<sub>3</sub> and Its 3-Sulfate in Newborn Plasma by LC/ESI-MS/MS after Derivatization with a Proton-Affinitive Cookson-Type Reagent

A Method for Simultaneous Determination of 25-Hydroxyvitamin D<sub>3</sub> and Its 3-Sulfate in Newborn Plasma by LC/ESI-MS/MS after Derivatization with a Proton-Affinitive Cookson-Type Reagent

Mass Spectrometric Profiling of Vitamin D Metabolites beyond 25-Hydroxyvitamin D

Sulfation of vitamin D3‐related compounds—identification and characterization of the responsible human cytosolic sulfotransferases

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Sulfation of vitamin D₃‐related compounds—identification and characterization of the responsible human cytosolic sulfotransferases