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

Higashi, Tatsuya; Shimada, Kaoru

doi:10.1002/bmc.3808

Cited by 22 publications

(12 citation statements)

References 71 publications

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“…The use of a derivatisation agent has remained an essential step, especially when analysed using entry-level to mid-range LC-MS/MS systems. The most commonly described derivatisation agents for vitamin D metabolites in the literature (reviewed in [59]) are based on a substituted form of 1,2,4-triazoline-3,5-dione (TAD) at the 4-position (4-X-TAD). The Diels-Alder reaction is stable, robust, can be performed under ambient conditions and terminated by the addition of water.…”

Section: 25(oh) 2 Dmentioning

confidence: 99%

Vitamin D Measurement, the Debates Continue, New Analytes Have Emerged, Developments Have Variable Outcomes

et al. 2019

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The demand for measurement of vitamin D metabolites for clinical diagnosis and to advance our understanding of the role of vitamin D in human health has significantly increased in the last decade. New developments in technologies employed have enabled the separation and quantification of additional metabolites and interferences. Also, developments of immunoassays have changed the landscape. Programmes and materials for assay standardisation, harmonisation and the expansion of the vitamin D external quality assurance scheme (DEQAS) with the provision of target values as measured by a reference measurement procedure have improved standardisation, quality assurance and comparability of measurements. In this article, we describe developments in the measurement of the commonly analysed vitamin D metabolites in clinical and research practice. We describe current analytical approaches, discuss differences between assays, their origin, and how these may be influenced by physiological and experimental conditions. The value of measuring metabolites beyond 25 hydroxyvitamin D (25(OH)D), the marker of vitamin D status, in routine clinical practice is not yet confirmed. Here we provide an overview of the value and application of the measurement of 1,25 dihydroxyvitamin D, 24,25 dihydroxyvitamin D and free 25OHD in the diagnosis of patients with abnormalities in vitamin D metabolism and for research purposes.

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Section: 25(oh) 2 Dmentioning

confidence: 99%

Vitamin D Measurement, the Debates Continue, New Analytes Have Emerged, Developments Have Variable Outcomes

et al. 2019

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“…Thus, there is an increasing demand for the quantitative and routine mass spectrometric measurement of differential VD metabolites . Because VD metabolites exhibit a low ionization efficiency under the conditions used in VD analysis by liquid chromatography/tandem mass spectrometry (LC/MS/MS), attempts to improve ionization efficiency by derivatization are being reported …”

Section: Introductionmentioning

confidence: 99%

A novel caged Cookson‐type reagent toward a practical vitamin D derivatization method for mass spectrometric analyses

Shimada

Sato

Takiwaki

et al. 2020

Rapid Comm Mass Spectrometry

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Rationale 25‐Hydroxylated vitamin D is the best marker for vitamin D (VD). Due to its low ionization efficiency, a Cookson‐type reagent, 1,2,4‐triazoline‐3,5‐dione (TAD), is used to improve the detection/quantification of VD metabolites by liquid chromatography/tandem mass spectrometry (LC/MS/MS). However, the high reactivity of TAD makes its solution stability low and inconvenient for practical use. We here describe the development of a novel caged Cookson‐type reagent, and we assess its performances in the quantitative and differential detection of four VD metabolites in serum using LC/MS/MS. Methods Caged 4‐(4′‐dimethylaminophenyl)‐1,2,4‐triazoline‐3,5‐dione (DAPTAD) analogues were prepared from 4‐(4′‐dimethylaminophenyl)‐1,2,4‐triazolidine‐3,5‐dione. Their stability and reactivity were examined. The optimized caged DAPTAD (14‐(4‐(dimethylamino)phenyl)‐9‐phenyl‐9,10‐dihydro‐9,10‐[1,2]epitriazoloanthracene‐13,15‐dione, DAP‐PA) was used for LC/MS/MS analyses of VD metabolites. Results The solution stability of DAP‐PA in ethyl acetate dramatically improved compared with that of the non‐caged one. We measured the thermal retro‐Diels‐Alder reaction enabling the release of DAPTAD and found that the derivatization reaction was temperature‐dependent. We also determined the detection limit and the lower limit of quantifications for four VD metabolites with DAPTAD derivatization. Conclusions DAP‐PA was stable enough for mid‐ to long‐term storage in solution. This advantage shall contribute to the detection and quantification of VD in clinical laboratories, and as such to the broader use of clinical mass spectrometry.

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“…erefore, it could not be quantified by UV or HPLC methods. On the other hand, LC-MS has been reported as a highly sensitive, fast, and versatile method for quantification of vitamin D compounds in biological fluids [11,12]. But, the application of LC-MS in directly characterizing alfacalcidol dissolution content is still confined due to poor ionization efficiency of API by electrospray ionization (ESI) source.…”

Section: Introductionmentioning

confidence: 99%

Quantification of Alfacalcidol Tablets Dissolution Content by Chemical Derivatization and LC-MS

Liu

Chen

Yuan

et al. 2020

Journal of Analytical Methods in Chemistry

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Application of liquid chromatography-mass spectrometry (LC-MS) in analyzing the content of alfacalcidol tablets dissolution faces big challenges due to the low amount of alfacalcidol in each tablet and the low ionization efficacy of the compound with electrospray ionization (ESI) or atmospheric-pressure chemical ionization (APCI). Here, extraction, derivatization, and LC-MS quantitation method have been developed and validated for measuring alfacalcidol tablets dissolution content. After alfacalcidol dissolution solution was extracted with dichloromethane to remove surfactant and inorganic salts, alfacalcidol was then derivatized via a Cookson reagent, 4-phenyl-1, 2, 4-triazoline-3, 5-dione (PTAD), under ambient conditions. Alfacalcidol derivative was successfully analyzed by LC-MS. Limit of detection (LOD) of the derivatized alfacalcidol was improved 100 times (0.01 μg/mL) compared with the nontreated compound (1 μg/mL). The new method was then validated following International Conference on Harmonization (ICH) guidance. The method shows a good linearity with r2 > 0.99. Interday and intraday reproducibility was 3.3% and 7.9%, respectively. This procedure can be used in quantification of alfacalcidol tablets dissolution content and corresponding pharmaceutical quality control.

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

Cited by 22 publications

References 71 publications

Vitamin D Measurement, the Debates Continue, New Analytes Have Emerged, Developments Have Variable Outcomes

Vitamin D Measurement, the Debates Continue, New Analytes Have Emerged, Developments Have Variable Outcomes

A novel caged Cookson‐type reagent toward a practical vitamin D derivatization method for mass spectrometric analyses

Quantification of Alfacalcidol Tablets Dissolution Content by Chemical Derivatization and LC-MS

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