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A simple and efficient derivatization strategy combined with switchable solvent liquid-liquid microextraction hydroxychloroquine methyl acetate-d3 -based quadruple isotope dilution gas chromatography mass spectrometry for the determination of hydroxychloroquine sulfate in biological fluids.
Erarpat, Sezin; Bodur, Süleyman; Öner, Miray; Günkara, Ömer Tahir; Bakirdere, Sezgin.
  • Erarpat S; Faculty of Art and Science, Chemistry Department, Yildiz Technical University, Istanbul, Turkey.
  • Bodur S; Faculty of Art and Science, Chemistry Department, Yildiz Technical University, Istanbul, Turkey.
  • Öner M; Faculty of Art and Science, Chemistry Department, Yildiz Technical University, Istanbul, Turkey.
  • Günkara ÖT; Faculty of Art and Science, Chemistry Department, Yildiz Technical University, Istanbul, Turkey.
  • Bakirdere S; Faculty of Art and Science, Chemistry Department, Yildiz Technical University, Istanbul, Turkey.
Rapid Commun Mass Spectrom ; 36(12): e9282, 2022 Jun 30.
Article in English | MEDLINE | ID: covidwho-1802571
ABSTRACT
RATIONALE A derivatization switchable solvent liquid-liquid microextraction quadruple isotope dilution gas chromatography mass spectrometry (D-SS-LLME-ID4 -GC/MS) method is presented for the determination of hydroxychloroquine sulfate in human biofluids.

METHODS:

While mixing type/period and concentration of NaOH were optimized via a univariate optimization approach, a multivariate optimization approach was used to determine optimum values for relatively more important parameters such as volumes of derivatization agent (acetic anhydride), NaOH and switchable solvent.

RESULTS:

Under the optimum experimental conditions, limit of detection and limit of quantification were calculated as 0.03 and 0.09 mg/kg (mass based), respectively. An isotopically labelled material (hydroxychloroquine methyl acetate-d3 ) was firstly synthesized to be used in ID4 experiments which give highly accurate and precise recovery results. After the application of D-SS-LLME-ID4 , superior percent recovery results were recorded as 99.9 ± 1.6-101.3 ± 1.2 for human serum, 99.9 ± 1.7-99.8 ± 1.8 for urine and 99.6 ± 1.5-101.0 ± 1.1 for saliva samples.

CONCLUSIONS:

The developed D-SS-LLME-ID4 -GC/MS method compensates the complicated matrix effects of human biofluids and provides highly accurate quantification of an analyte with precise results.
Subject(s)

Full text: Available Collection: International databases Database: MEDLINE Main subject: Liquid Phase Microextraction Limits: Humans Language: English Journal: Rapid Commun Mass Spectrom Year: 2022 Document Type: Article Affiliation country: Rcm.9282

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Full text: Available Collection: International databases Database: MEDLINE Main subject: Liquid Phase Microextraction Limits: Humans Language: English Journal: Rapid Commun Mass Spectrom Year: 2022 Document Type: Article Affiliation country: Rcm.9282