Mechanism of error caused by isotope-labeled internal standard: accurate method for simultaneous measurement of vitamin D and pre-vitamin D by liquid chromatography/tandem mass spectrometry

Huang, Min; Cadwallader, Amy B.; Heltsley, Rebecca

doi:10.1002/rcm.6987

Cited by 12 publications

(6 citation statements)

References 13 publications

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“…SIL-IS was seldom used in previous assays of cefaclor quantification in human plasma (Chen et al, 2003(Chen et al, , 2012Huang, Cadwallader, & Heltsley, 2014;Jiang et al, 2009;Kai et al, 2003;Koytchev et al, 2004;Li et al, 2010;Lindgren, 1987;Naz et al, 2017;Qu et al, 2022;Tutunji et al, 2001). As an ideal method for precise quantification using LC-ESI-MS/MS (Huang, Cadwallader, & Heltsley, 2014), SIL-IS has almost similar physical and chemical properties, retention times, and ionization to the analyte (Liu et al, 2019;Loos et al, 2016). It can eliminate matrix effect.…”

Section: Pharmacokinetics Studymentioning

confidence: 99%

“…It can eliminate matrix effect. Besides, the extraction and elution procedures of SIL-IS and the analyte are quite similar (Huang, Cadwallader, & Heltsley, 2014). SIL-IS simplifies the quantification of analytes, rendering the determination results more reliable and accurate (Loos et al, 2016).…”

Section: Pharmacokinetics Studymentioning

confidence: 99%

“…ter meet the requirements of therapeutic drug monitoring (TDM) and pharmacokinetics evaluation. Compared with the reported method(Huang, Cadwallader, & Heltsley, 2014), the detection efficiency was greatly improved with a total run time of only 2.3 min. Because of the slight acidity of cefaclor, formic acid was added to the mobile phase in this study to enhance the signal strength of cefaclor and SIL-IS,T A B L E 4Abbreviation: CV, coefficient of variation.…”

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confidence: 92%

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Quantification of cefaclor in human plasma using SIL‐IS LC‐ESI‐MS/MS for pharmacokinetics study in healthy Chinese volunteers

Chen

Liu

Wang

et al. 2023

Biomedical Chromatography

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A steady, high‐efficiency, and precise liquid chromatography‐electrospray ionization‐tandem mass spectrometry method was established and validated using cefaclor‐d5 as the stable isotope‐labeled internal standard for quantification of cefaclor in human plasma. One‐step protein precipitation was applied to extract human plasma samples using methanol as precipitant. An Ultimate XB C18 column (2.1 × 50.0 mm, 5.0 μm) was used to achieve chromatographic separation. Mobile phases of gradient elution were an aqueous solution containing 0.1% formic acid (mobile phase A) and an acetonitrile solution containing 0.1% formic acid (mobile phase B). Electrospray ionization in positive‐ion mode was applied to detect under multiple reaction monitoring mode. Target fragment ion pairs of cefaclor and stable isotope‐labeled internal standard, respectively, were m/z 368.2 → 191.1 and m/z 373.2 → 196.1. Linear range of this method was between 20.0 and 10,000.0 ng/ml, with coefficient of determination (R2) >0.9900. Seven concentrations of quality control samples were used: 20.0 ng/ml (lower limit of quantitation), 60.0 ng/ml (low quality control), 650 ng/ml (middle quality control), 5000 ng/ml (arithmetic average middle quality control [AMQC]), 7500 ng/ml (high quality control), 10,000 ng/ml (upper limit of quantification), and 40,000 ng/ml (dilution quality control [DQC]). The method was validated for selectivity, lower limit of quantitation, linearity, accuracy, precision, recovery, matrix effect, dilution reliability, stability, carryover, and incurred sample reanalysis. This stable isotope‐labeled internal standard liquid chromatography‐electrospray ionization‐tandem mass spectrometry approach has been successfully applied to study the pharmacokinetics of cefaclor dry suspension among healthy Chinese volunteers.

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Section: Pharmacokinetics Studymentioning

confidence: 99%

Section: Pharmacokinetics Studymentioning

confidence: 99%

mentioning

confidence: 92%

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Quantification of cefaclor in human plasma using SIL‐IS LC‐ESI‐MS/MS for pharmacokinetics study in healthy Chinese volunteers

Chen

Liu

Wang

et al. 2023

Biomedical Chromatography

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“…Эти методы легко автоматизируются, с их помощью можно проводить анализ одновременно большого количества проб, и они широко распространены к клинической практике. Однако эти методы анализа имеют свои недостатки, они не совсем пригодны для определения стероидных гормонов (тестостерон, эстрадиол), к числу стероидов относится и витамин D. Стандартом определения общего витамина D в сыворотке крови служит метод тандем-масс-спектрометрии LC/MS/MS [13].…”

Section: The Classic Function Of Vitamin D Is To Regulate Calcium Metabolism Currently However Convincing Data Have Been Obtained On the unclassified

Clinical significance and features of laboratory determination of vitamin D

Дрыгина

2020

Medicinskij alfavit

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The classic function of vitamin D is to regulate calcium metabolism. Currently, however, convincing data have been obtained on the relationship of vitamin D deficiency with the development of a number of diseases. The article analyzes the results of recent studies that present the effects of vitamin D on the immune system, cardiovascular system and liver diseases. Discusses the mechanisms of admission of vitamin D in the body, presents new data on the regulation of levels of active form of vitamin D phosphatonins (FGF23, MEPE, sFRP-4) and protein Klotho. The characteristic of methods of determination of vitamin D in blood serum is presented. Biological factors that influence the results of quantitative determination of vitamin D with different methods are considered separately.

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“…LC-MS/MS (liquid chromatography tandem mass spectrometry) is the best technique currently available for quantitation of Vitamin D3, D2 and their 25-OH derivatives 25OHD3 and 25OHD2 6,7 in feed, serum and related matrices especially in that it does not suffer most of the limitations inherent to immunoassays such as low specificity. Use of Atmospheric Pressure Chemical Ionization (APCI) avoids the need for derivatization, 8 whereas the more commonly used Electrospray Ionization (ESI) requires a variety of Diels-Alder type derivatization methodologies; 9–13 see reviews. 14–16 Both techniques suffer from matrix effects.…”

Section: Introductionmentioning

confidence: 99%

Vitamin D analyses in veterinary feeds by gas chromatography-tandem mass spectrometry

Lehner

Johnson

Zimmerman

et al. 2021

Eur J Mass Spectrom (Chichester)

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This report examines the feasibility of determination of Vitamin D3, D2 and their 25-hydroxy metabolites utilizing Gas Chromatography Tandem Mass Spectrometry (GC/MS/MS) as a potential alternative to popular Liquid Chromatography Tandem Mass Spectrometric (LC/MS/MS) methodologies. The GC/MS/MS approach was found to operate reasonably well despite long-standing concerns that gas-liquid chromatography of vitamin D compounds invoke thermal rearrangements owing to the relatively high inlet and capillary column temperatures used. The workup procedure involved incubation of feed samples with concentrated potassium hydroxide for overnight fat saponification, extraction of D Vitamins in n-hexane and reaction with N,O-bis(trimethylsilyl)trifluoroacetamide at 70 °C for 30 mins. In addition to parent compounds, small amounts of pyro-, isopyro-, and iso-vitamin D and isotachysterol3 variants were obtained from each Vitamin D-related compound upon extraction and GC/MS/MS analysis. Mass spectral and chromatographic behavior of these compounds are herein described and interpreted. Multiple Reaction Monitoring settings on GC/MS/MS included m/z 456→351 for Vitamin D3 and m/z 486→363 for Vitamin D2. Trimethylsilylation enabled single predominant peaks for Vitamins D3 and D2, and sample workup in the presence of deuterated Vitamin D analogs enabled accurate and precise sensitivity to 1 ppb (ng/g) in feeds. The method could be extended with reasonable accuracy to 25-hydroxy (25OH) compounds, but accuracies would be significantly improved by inclusion of respective 25OH-specific deuterated internal standards. The method was applied to 27 submissions of suspect dog foods of which 22% were discovered elevated and 44% were discovered to contain toxic levels of Vitamin D3. The described method was thus discovered to provide a suitable mass spectrometric approach for Vitamin D, proving itself here specifically of value in detection of ergocalciferol and cholecalciferol in animal feeds. The specificity and sensitivity of the tandem quadrupole approach can enable suitable applicability to serum determination if desired.

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Mechanism of error caused by isotope-labeled internal standard: accurate method for simultaneous measurement of vitamin D and pre-vitamin D by liquid chromatography/tandem mass spectrometry

Cited by 12 publications

References 13 publications

Quantification of cefaclor in human plasma using SIL‐IS LC‐ESI‐MS/MS for pharmacokinetics study in healthy Chinese volunteers

Quantification of cefaclor in human plasma using SIL‐IS LC‐ESI‐MS/MS for pharmacokinetics study in healthy Chinese volunteers

Clinical significance and features of laboratory determination of vitamin D

Vitamin D analyses in veterinary feeds by gas chromatography-tandem mass spectrometry

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