Vitamin D metabolite profiling using liquid chromatography–tandem mass spectrometry (LC–MS/MS)

Jones, Glenville; Kaufmann, Martin

doi:10.1016/j.jsbmb.2015.09.026

Cited by 53 publications

(27 citation statements)

References 27 publications

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“…The derivatization with a Cookson‐type reagent is a key step for the robust and sensitive analysis of VD compounds using LC/MS(/MS) as cited in recently published articles (Kassim, Gomes, Shaw, & Hewavitharana, ; He et al, ) and reviews (Jones & Kaufmann, ; Volmer, Mendes, & Stokes, ). The details of the sensitivity of the derivatized VD metabolites are summarized in the review by Higashi and Ogawa ().…”

Section: Application Of Cookson‐type Reagents To Analysis Of Vd Compomentioning

confidence: 99%

“…Although the determination of the major D 3 metabolites [25(OH)D 3 , 24,25(OH) 2 D 3 , 1,25(OH) 2 D 3 ] in human plasma using HPLC/FL with the DMEQTAD-derivatization was reported byWang, Shimizu, Numano, Asaoka, and Yamada (1997), tedious and time-consuming pretreatment procedures, including preparative HPLC, were necessary before the derivatization and a long chromatographic run time (>30 min) was also required for the separation of the analytes from the interfering compounds. Basically, HPLC with UV or FL is rarely used today for the determination of VD compounds in biological samples, which has been transferred to LC/MS(/MS).The derivatization with a Cookson-type reagent is a key step for the robust and sensitive analysis of VD compounds using LC/MS(/ MS) as cited in recently published articles(Kassim, Gomes, Shaw, & Hewavitharana, 2016;He et al, 2016) and reviews(Jones & Kaufmann, 2016;Volmer, Mendes, & Stokes, 2015). The details of the sensitivity of the derivatized VD metabolites are summarized in the review byHigashi and Ogawa (2016a).…”

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Application of Cookson‐type reagents for biomedical HPLC and LC/MS analyses: a brief overview

Higashi

Shimada

2016

Biomedical Chromatography

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High-performance liquid chromatography (HPLC), LC/mass spectrometry (MS) and LC/tandem mass spectrometry (MS/MS) have been widely used for biomedical analyses, in which chemical derivatization is one of the most important methods to increase the sensitivity and selectivity. A Cookson-type reagent [4-substituted-1,2,4-triazoline-3,5-dione (4-substituted-TAD)] reacts with the compound bearing a conjugated diene, such as the vitamin D compound, to quantitatively form the stable Diels-Alder adduct. The reagent with a chromophore or fluorophore at the 4-position of TAD yields a highly responsive adduct for the UV or fluorescence detection, respectively. The Diels-Alder adduct with a Cookson-type reagent having a permanently charged, proton-affinitive or electron-affinitive moiety is sensitively detected by a specific MS analyzer. This paper is a brief overview of the applications of the reagents for biomedical analyses mainly using HPLC or LC/MS(/MS).

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Section: Application Of Cookson‐type Reagents To Analysis Of Vd Compomentioning

confidence: 99%

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confidence: 99%

Application of Cookson‐type reagents for biomedical HPLC and LC/MS analyses: a brief overview

Higashi

Shimada

2016

Biomedical Chromatography

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“…However, it is still difficult to quantify the low endogenous levels of 1,25(OH) 2 VitD in small sample volumes. In an attempt to further increase the method sensitivity, new effective dienophiles, 4-(4′-dimethylaminophenyl)-1,2,4-triazoline-3,5-dione; 4-[2-(3,4-dihydro-6,7-dimethoxy-4-methyl-3-oxo-2-quinoxalinyl)ethyl]-3H-1,2,4-triazole-3,5(4H)-dione; and other "triazolinediones," have been developed (25,(33)(34)(35)(36)(37). Among them, the positively charged derivatization reagent, Amplifex-Diene and SecoSET, are reported to have a 10-fold ioniziation efficiency improvement over PTAD (25,36,38).…”

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confidence: 99%

A new sensitive LC/MS/MS analysis of vitamin D metabolites using a click derivatization reagent, 2-nitrosopyridine

Wan

Yang

Barnych

et al. 2017

Journal of Lipid Research

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This article is available online at http://www.jlr.orgIn 1943, vitamin D was recommended as an essential nutrient for the US public. People can acquire the precursors to the bioactive forms, vitamin D 3 and vitamin D 2 , from diet, supplements, and sunlight. In the liver, both forms of vitamin D are rapidly hydroxylated to corresponding 25-hydroxyvitamin D [25(OH)VitD]. Being a predominant metabolite, circulating 25(OH)VitD serves as the preferred surrogate biomarker of vitamin D nutritional status (1, 2). Low levels of 25(OH)VitD indicate low vitamin D nutritional intake, which is related to many diseases, such as osteomalacia, multiple sclerosis, Parkinson's disease, asthma, and other health risks, including muscle weakness, diabetes, and cognitive decline or Alzheimer's disease (3-7). Consequently, analytical techniques for measurement of 25(OH)VitD have been developed (8)(9)(10)(11)(12). In the kidney, 25(OH)VitD is further hydroxylated to 1,25-dihydroxyvitamin D [1,25(OH) 2 VitD]. 1,25(OH) 2 VitD is the major biologically active metabolite and plays an important role in decreasing the risk of many diseases, including common cancers, cardiovascular disease, autoimmune disease, and chronic kidney disease (13)(14)(15)(16)(17). Most recently, we have demonstrated that 1,25(OH) 2 VitD also appears to be important for the health of the eye (18). The influence that these biologically active forms of vitamin D have on these numerous diseases and associated organ systems 23 January 2017. Published, JLR Papers in Press, February 1, 2017 DOI 10.1194 26,26,27,27,(OH)VitD 3 ; ALTM, all laboratory trimmed mean; CUDA, 12-(3-cyclohexyl-ureido)-dodecanoic acid; DEQAS, Vitamin D External Quality Assessment Scheme; LLE-SPE, liquid-liquid extraction followed by solid-phase extraction; LLOQ, lower limit of quantification; MRM, multiple reaction monitoring; PTAD, 4-phenyl-1,2,4-triazole-3,5-dione; PyrNO, 2-nitrosopyridine; QC, quality control. This work was supported by the National Institutes of Health/National Eye Institute grant R01 EY021747 (to M.A.W.), National Institute of Environmental Health Sciences (NIEHS) grant R01 ES002710, NIEHS Superfund Research Program grant P42 ES004699 (to B.D.H.), the West Coast Metabolomics Center at UC Davis (National Institutes of Health/National Institute of Diabetes and Digestive and Kidney Diseases grant U24 DK097154), and National Institutes of Health/NIEHS grant 1K99ES024806-01 (to K.S.S.L.). Manuscript received 22 November 2016 and in revised form

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“…Sophisticated methodologies for 25-(OH) D measurements include enzyme linked immunosorbent assay, 9) chemiluminescence assay, 9,10) GC-MS, 11) HPLC-UV detection, 12,13) radio immunoassay 14,15) and LC-MS/MS. [16][17][18][19] LC-MS/MS technique is the gold standard technique for the determination of 25-(OH) D. It entails high end expensive instrumentation and skilled technical labor. Ion suppression from matrix effects, interference from the C3 epimer and mandated derivatization to increase ionization are the other well-known drawbacks limiting the use of this technique.…”

Section: Introductionmentioning

confidence: 99%

Cost-Effective HPLC-UV Method for Quantification of Vitamin D<sub>2</sub> and D<sub>3</sub> in Dried Blood Spot: A Potential Adjunct to Newborn Screening for Prophylaxis of Intractable Paediatric Seizures

Mathew

Moorkoth

Rane

et al. 2019

CHEMICAL & PHARMACEUTICAL BULLETIN

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25-Hydroxyvitamin D (25-(OH)D) deficiency is recently been described as one of the multiple factors responsible for pediatric seizures. 25-Hydroxyvitamin D3 and 25-Hydroxyvitamin D2 are the well-known markers to determine Vitamin D status. In this work we report the development of a sensitive and cost effective HPLC technique for the quantification of the vitamin D metabolites from dried blood spot samples (DBS). The metabolites were extracted using acetonitrile-methanol-0.1% formic acid (60 : 20 : 20 (v/v)) and analyzed on an Acclaim C 18 column (150 4.6 mm i.d., 3 µm) at a flow rate of 1 mL/min. The method was linear in the range of 10-80 ng/mL. Limit of detection and limit of quantification (LOQ) of the method were 5 and 10 ng/mL respectively. Extensive stability studies demonstrated the analytes to be stable in stock and matrix with a percent change within the acceptable range of 15%. Comparison of the newly developed HPLC-DBS method with the reported LC-MS-DBS and electrochemiluminescence immunoassay (ECLIA) methods followed by Bland-Altman analysis demonstrated a bias of 0.08 and 0.14, respectively proving the methods are comparable. Application of the developed method to a pediatric seizure cohort depicted 46.6% of cases as deficient and 26.6% as insufficient for 25-(OH)D. Among deficient cases 8 samples were below 10 ng/mL and exact amount was not calculated since these were below the LOQ levels. The mean standard deviation (S.D.) in the remaining 6 deficient cases was 13.22 2.80 ng/mL. The levels in healthy infants were 33.9 6.11 ng/mL. The method can be used routinely for assessing 25-(OH)D deficiency in newborn.

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Vitamin D metabolite profiling using liquid chromatography–tandem mass spectrometry (LC–MS/MS)

Cited by 53 publications

References 27 publications

Application of Cookson‐type reagents for biomedical HPLC and LC/MS analyses: a brief overview

Application of Cookson‐type reagents for biomedical HPLC and LC/MS analyses: a brief overview

A new sensitive LC/MS/MS analysis of vitamin D metabolites using a click derivatization reagent, 2-nitrosopyridine

Cost-Effective HPLC-UV Method for Quantification of Vitamin D<sub>2</sub> and D<sub>3</sub> in Dried Blood Spot: A Potential Adjunct to Newborn Screening for Prophylaxis of Intractable Paediatric Seizures

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