Quantification of acitretin in human plasma by microbore liquid chromatography—negative chemical ionization mass spectrometry

Fayer, B.E.; Huselton, Christine; Garland, William A.; Liberato, Daniel J.

doi:10.1016/0378-4347(91)80347-f

Cited by 14 publications

(11 citation statements)

References 17 publications

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“…Historically only a handful of articles have described the use of LC-MS for the determination of retinoids in biological samples (Eckhoff et al, 1990;Fayer et al, 1991;Ranalder et al, 1993;Bempong et al, 1995). During the last decade however, modern soft atmospheric pressure ionization techniques like electrospray (ESI) and atmospheric pressure chemical ionization (APCI) have been explored for retinoid analysis.…”

Section: Liquid Chromatography-mass Spectrometry (Lc-ms)mentioning

confidence: 99%

Methods for detecting and identifying retinoids in tissue

Gundersen

2006

J. Neurobiol.

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Methods for retinoid analysis in tissue include direct spectrophotometry or fluorometry and retinoid responsive reporter constructs in the form of cell reporter assays or transgenic reporter animals, but chromatographic methods dominate and posses several superior features in quantitative analysis. The multitude of extraction protocols used can coarsely be divided into manual liquid-liquid extraction protocols and semi-or fully automated solid phase extraction-based protocols.Liquid chromatographic separation in reversed phase dominates although normal phase is also used. Detection is mainly performed with UV detectors although electrochemical and fluorescence detection is also used. Mass spectrometry in combination with LC is more often used in retinoid analysis and is likely to dominate in the future.

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Section: Liquid Chromatography-mass Spectrometry (Lc-ms)mentioning

confidence: 99%

Methods for detecting and identifying retinoids in tissue

Gundersen

2006

J. Neurobiol.

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“…Fayer et al . (1991) reported plasma concentrations of acitretin and 13‐ cis ‐acitretin with linearity range 1–20 ng/mL without addressing the detailed stability performance and matrix effect evaluation. Interference from endogenous matrix compounds would distort acitretin and active metabolite bioanalysis.…”

Section: Introductionmentioning

confidence: 99%

“…Several approaches for acitretin and active metabolite quantification in plasma using HPLC/UV have either lacked sensitivity or involved tedious extraction steps leading to poor recovery or matrix suppression with no precautionary measure to arrest photoisomerization/interconversion (Wyss and Bucheli, 1992;Gunderson et al, 1997;Surber et al, 1992;Decker and Zimmerman, 1995;Leenheer et al, 1990). Fayer et al (1991) reported plasma concentrations of acitretin and 13-cis-acitretin with linearity range 1-20 ng/mL without addressing the detailed stability performance and matrix effect evaluation. Interference from endogenous matrix compounds would distort acitretin and active metabolite bioanalysis.…”

Section: Introductionmentioning

confidence: 99%

Stability‐indicating validation of acitretin and isoacitretin in human plasma by LC‐ESI‐MS/MS bioanalytical method and its application to pharmacokinetic analysis

Kumar¹,

Monif²,

Khuroo³

et al. 2010

Biomedical Chromatography

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LC- ESI- MS/MS simultaneous bioanalytical method was developed to determine acitretin and its metabolite isoacitretin in human plasma using acitretin-d3 used as the internal standard for both analytes. The compounds were extracted using protein precipitation coupled with liquid-liquid extraction with flash freezing technique. Negative mass transitions (m/z) of acitretin, isoacitretin and acitretin-d3 were detected in multiple reactions monitoring (MRM) mode at 325.4 → 266.3, 325.2 → 266.1 and 328.3 → 266.3, respectively, with a turbo ion spray interface. The chromatographic separation was achieved on an Ascentis-RP amide column (4.6 × 150 mm, 5 µm) with mobile phase delivered in isocratic mode. The method was validated over a concentration range of 1.025-753.217 ng/mL for acitretin and 0.394-289.234 ng/mL for isoacitretin with a limit of quantification of 1.025 and 0.394 ng/mL. The intra-day and inter-day precisions were below 8.1% for acitretin and below 13.8% for isoacitretin, while accuracy was within ±7.0 and ±10.6% respectively. For the first time, the best possible conditions for plasma stability of acitretin and isoacitretin are presented and discussed with application to clinical samples.

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“…The combination of high‐performance liquid chromatography and mass spectrometry (HPLC/MS) is a powerful analytical technique that combines the resolving power of HPLC with the detection specificity and potentially low detection limits of MS. Historically, there have been a number of papers that describe the use of LC/MS for the determination of retinoids in biological samples 4–17. During the last decade modern soft atmospheric pressure ionization techniques like electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) have been explored for retinoid analysis 5, 6, 8–17.…”

mentioning

confidence: 99%

Quantitative high‐throughput determination of endogenous retinoids in human plasma using triple‐stage liquid chromatography/tandem mass spectrometry

Gundersen

Bastani

Blomhoff

2007

Rapid Comm Mass Spectrometry

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A high-throughput ultrasensitive analytical method based on liquid chromatography with positive ion atmospheric pressure chemical ionization (APCI) coupled to tandem mass spectrometric detection (LC/MS/MS) was developed for the determination of all-trans-4-oxo-retinoic acid (at4oxoRA), 13-cis-4-oxo-retinoic acid (13c4oxoRA), 13-cis-retinoic acid (13cRA), all-trans-retinoic acid (atRA) and all-trans-retinol (atROH) in human plasma. A stable isotope of atRA was used as internal standard (IS). The analytes and IS were isolated from 100 microL plasma by acetonitrile mono-phase extraction (MPE) performed in black 96-well microtiterplates. A 100 microL injection was focused on-column and chromatographed on an Agilent ZORBAX SB-C18 rapid-resolution high-throughput (RRHT) column with 1.8-microm particles (4.6 mmx50 mm) maintained at 60 degrees C. The initial mobile phase composition was acetonitrile/water/formic acid (10:90:0.1, v/v/v) delivered at 1.8 mL/min. Elution was accomplished by a fast gradient to acetonitrile/methanol/formic acid (90:10:0.1, v/v/v). The method had a chromatographic total run time of 7 min. An Applied Biosystems 4000 Q TRAP linear tandem mass spectrometer equipped with a heated nebulizer (APCI) ionization source was operated in multiple reaction monitoring (MRM) mode with the precursor-to-product ion transitions m/z 315.4-->297 (4-oxo-retinoic acids), 301.2-->205 (retinoic acids), 305.0-->209 (IS) and 269.2-->93 (retinol) used for quantification. The assay was fully validated and found to have acceptable accuracy, precision, linearity, sensitivity and selectivity. The mean extraction recoveries from spiked plasma samples were 80-105% for the various retinoids at three different levels. The intra-day accuracy of the assay was within 8% of nominal and intra-day precision was better than 8% coefficient of variance (CV) for retinoic acids. Inter-day precision results for quality control samples run over a 12-day period alongside clinical samples showed mean precision better than 12.5% CV. The limit of quantification was in the range of 0.1-0.2 ng/mL and the mass limit of detection (mLOD) was in the range 1-4 pg on column for the retinoic acids. The assay has been successfully applied to the analysis of 1700 plasma samples.

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Quantification of acitretin in human plasma by microbore liquid chromatography—negative chemical ionization mass spectrometry

Cited by 14 publications

References 17 publications

Methods for detecting and identifying retinoids in tissue

Methods for detecting and identifying retinoids in tissue

Stability‐indicating validation of acitretin and isoacitretin in human plasma by LC‐ESI‐MS/MS bioanalytical method and its application to pharmacokinetic analysis

Quantitative high‐throughput determination of endogenous retinoids in human plasma using triple‐stage liquid chromatography/tandem mass spectrometry

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