Accurate and sensitive determination of hydroxychloroquine sulfate used on COVID-19 patients in human urine, serum and saliva samples by GC-MS

Bodur, Süleyman; Erarpat, Sezin; Günkara, Ömer Tahir; Bakırdere, Sezgin

doi:10.1016/j.jpha.2021.01.006

Cited by 21 publications

(16 citation statements)

References 32 publications

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“…In addition, HCQ inhibits the synthesis of cytokines and reduces autophagy and lysosomal activity in host cells, all of which have immunomodulatory effects. [ 23 , 24 ] In general, hyphenated and electroanalytical techniques which including spectrophotometry, [ 25 ] high performance liquid chromatography, [ 26 , 27 , 28 , 29 ] gas chromatography mass spectrometry [ 30 ] potentiometry, [ 31 ] voltammetry, [ 32 , 33 ] are used to qualify and quantify HCQ. Both FPV and HCQ are reported in many guidelines for the treatment of COVID‐19.…”

Section: Introductionmentioning

confidence: 99%

Quantitative analysis of favipiravir and hydroxychloroquine as FDA‐approved drugs for treatment of COVID‐19 using synchronous spectrofluorimetry: application to pharmaceutical formulations and biological fluids

et al. 2022

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Coronavirus disease 2019 (COVID‐19) is a contagious viral infection caused by coronavirus 2 (SARS‐CoV‐2) that causes severe acute respiratory syndrome. It has ravaged several countries and burdened many healthcare systems. As the process of authorizing a novel treatment for human use is extensive and involves multiple phases to obtain safety information and identify potential concerns. Therefore, the fastest and easiest choice was to use United States Food and Drug Administration (US FDA)‐approved drugs such as favipiravir and hydroxychloroquine. For the simultaneous estimation of both medications, a simple synchronous spectrofluorimetric approach was established in which both drugs were measured at 372 and 323 nm, respectively in the presence of each other without interference at Δλ 60 nm. The effect of various experimental conditions on synchronous fluorescence intensities were thoroughly investigated and optimized. The maximum synchronous fluorescence intensities were obtained at pH 5.4 using acetate buffer (0.2 M, 0.5 ml) and ethanol as a diluent. Excellent linearity ranges were obtained using 1.0–18.0 ng/ml and 10.0–120.0 ng/ml for favipiravir and hydroxychloroquine, respectively. The approach exhibited high sensitivity with detection limits down to 0.25 ng/ml and 1.52 ng/ml and quantitation limits down to 0.77 ng/ml and 4.62 ng/ml, respectively. Spiking human plasma samples with the studied drugs yielded high % recoveries, allowing a significant bioanalytical application. Moreover, the method was validated according to International Conference on Harmonization guidelines and further applied to commercial pharmaceutical preparations with good results.

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Section: Introductionmentioning

confidence: 99%

Quantitative analysis of favipiravir and hydroxychloroquine as FDA‐approved drugs for treatment of COVID‐19 using synchronous spectrofluorimetry: application to pharmaceutical formulations and biological fluids

et al. 2022

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“…Therefore, identification and quantification of hydroxychloroquine in biological samples are significant steps for the evaluation of its effects on human health. In the literature, various electroanalytic and chromatographic methods such as potentiometry, 14 differential pulse voltammetry, 15 square‐wave voltammetry, 16 high‐performance liquid chromatography (HPLC) with fluorometric detection, 17 HPLC with ultraviolet detection, 18 liquid chromatography–high‐resolution mass spectrometry, 19 liquid chromatography–tandem mass spectrometry 20 and gas chromatography–mass spectrometry (GC/MS) 21,22 have been reported for hydroxychloroquine determination in various samples. It is known that GC has widespread usage area due to its advantages such as good resolution, wide dynamic range, high sensitivity and selectivity 23 .…”

Section: Introductionmentioning

confidence: 99%

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

Bodur

Öner

et al. 2022

Rapid Comm Mass Spectrometry

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quadruple isotope dilution gas chromatography mass spectrometry (D-SS-LLME-ID 4 -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-d 3 ) was firstly synthesized to be used in ID 4 experiments which give highly accurate and precise recovery results. After the application of D-SS-LLME-ID 4 , 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-ID 4 -GC/MS method compensates the complicated matrix effects of human biofluids and provides highly accurate quantification of an analyte with precise results.

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“…For these reasons, developing a DLLME method for favipiravir determination was recommended. Although DLLME has been used to extract other Covid‐19 targeted medicines (Bodur et al, 2021a, 2021b), to the best of our knowledge, it has not been applied to favipiravir. In this work, gadolinium‐based MIL (Figure 1) was used for the DLLME of favipiravir from human plasma.…”

Section: Introductionmentioning

confidence: 99%

A gadolinium‐based magnetic ionic liquid for supramolecular dispersive liquid–liquid microextraction followed by HPLC/UV for the determination of favipiravir in human plasma

Abdallah

Hammad

Bedair

et al. 2022

Biomedical Chromatography

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Favipiravir is a potential antiviral medication that has been recently licensed for Covid-19 treatment. In this work, a gadolinium-based magnetic ionic liquid was prepared and used as an extractant in dispersive liquid-liquid microextraction (DLLME) of favipiravir in human plasma. The high enriching ability of DLLME allowed the determination of favipiravir in real samples using HPLC/UV with sufficient sensitivity.The effects of several variables on extraction efficiency were investigated, including type of extractant, amount of extractant, type of disperser and disperser volume. The maximum enrichment was attained using 50 mg of the Gd-magnetic ionic liquid (MIL) and 150 μl of tetrahydrofuran. The Gd-based MIL could form a supramolecular assembly in the presence of tetrahydrofuran, which enhanced the extraction efficiency of favipiravir. The developed method was validated according to US Food and Drug Administration bioanalytical method validation guidelines. The coefficient of determination was 0.9999, for a linear concentration range of 25 to 1.0 Â 10 5 ng/ml. The percentage recovery (accuracy) varied from 99.83 to 104.2%, with RSD values (precision) ranging from 4.07 to 11.84%. The total extraction time was about 12 min and the HPLC analysis time was 5 min. The method was simple, selective and sensitive for the determination of favipiravir in real human plasma.

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Accurate and sensitive determination of hydroxychloroquine sulfate used on COVID-19 patients in human urine, serum and saliva samples by GC-MS

Cited by 21 publications

References 32 publications

Quantitative analysis of favipiravir and hydroxychloroquine as FDA‐approved drugs for treatment of COVID‐19 using synchronous spectrofluorimetry: application to pharmaceutical formulations and biological fluids

Quantitative analysis of favipiravir and hydroxychloroquine as FDA‐approved drugs for treatment of COVID‐19 using synchronous spectrofluorimetry: application to pharmaceutical formulations and biological fluids

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

A gadolinium‐based magnetic ionic liquid for supramolecular dispersive liquid–liquid microextraction followed by HPLC/UV for the determination of favipiravir in human plasma

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Accurate and sensitive determination of hydroxychloroquine sulfate used on COVID-19 patients in human urine, serum and saliva samples by GC-MS

Cited by 21 publications

References 32 publications

Quantitative analysis of favipiravir and hydroxychloroquine as FDA‐approved drugs for treatment of COVID‐19 using synchronous spectrofluorimetry: application to pharmaceutical formulations and biological fluids

Quantitative analysis of favipiravir and hydroxychloroquine as FDA‐approved drugs for treatment of COVID‐19 using synchronous spectrofluorimetry: application to pharmaceutical formulations and biological fluids

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

A gadolinium‐based magnetic ionic liquid for supramolecular dispersive liquid–liquid microextraction followed by HPLC/UV for the determination of favipiravir in human plasma

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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