Enantioselective determination of chloroquine and its <i>n</i>‐dealkylated metabolites in plasma using liquid‐phase microextraction and LC‐MS

Magalhães, Igor Rafael dos Santos; Bonato, Pierina Sueli

doi:10.1002/jssc.200800320

Cited by 17 publications

(3 citation statements)

References 34 publications

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“…HPLC, which contains an UV detector, has been widely used. In addition, HPLC-DAD, [30,[45][46][47][48][49] , HPLC-fluorescence detection (FLD), [50][51][52][53][54][55][56][57] and HPLC-MS or HPLC-MS/MS systems [37,[58][59][60][61][62][63][64][65][66][67][68] are also widely preferred.…”

Section: Introductionmentioning

confidence: 99%

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Analytical Methods on Determination in Pharmaceuticals and Biological Materials of Chloroquine as Available for the Treatment of COVID-19

Saka

2020

Critical Reviews in Analytical Chemistry

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With the outbreak caused by the severe acute respiratory syndrome coronavirus (COVID-19), people's health and existing economies on a global scale are seriously threatened. Currently, most of the countries all over the world are studying extensively to better understand the antimalarial chloroquine (CQ) and hydroxychloroquine (HCQ) for therapeutic purposes due to the COVID-19 outbreak. However, CQ and HCQ can have serious side effects, from psychiatric effects to sudden death. Therefore, a faster and more effective detection method is needed to monitor drug concentrations. In this review, a large study was conducted on the detection techniques and quantitative determination methods of CQ and its related metabolites. In this review, chromatography, electrophoresis, electroanalytical, spectroscopic, and immunological methods for CQ and related metabolites are discussed extensively. It is hoped that a better understanding of the CQ used for therapeutic purposes in the COVID-19 outbreak will be provided.

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Section: Introductionmentioning

confidence: 99%

“…An LC-MS-MS method with three-phase liquid-phase microextraction (LPME) in plasma samples was developed for the enantioselective determination of CQ and n-dealkylated metabolites. [68] MS detection includes MRM with ESI in positive ion mode. Linearity was achieved above 5-500 ng/mL.…”

Section: Introductionmentioning

confidence: 99%

Analytical Methods on Determination in Pharmaceuticals and Biological Materials of Chloroquine as Available for the Treatment of COVID-19

Saka

2020

Critical Reviews in Analytical Chemistry

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“…Among high-performance separation techniques, HPLC is the most matured, universal, robust, sensitive, selective, and, therefore, the most frequently used technique (also) for the analysis of drugs and their metabolites in biological samples, as it can be seen from many application examples, see e.g. [1,2,[8][9][10][11][12][13][14][15][16][17]]. An analysis of recent trends indicates that CE can show real advantages over chromatographic methods in area of enantioselective analysis of low molecular ionic and, in some cases, also neutral compounds such as drugs, their metabolites, biomarkers, etc., present in complex matrices such as biological samples [3][4][5][6][7]18].…”

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confidence: 99%

Advanced CE for chiral analysis of drugs, metabolites, and biomarkers in biological samples

Mikuš

Maráková

2009

Electrophoresis

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An analysis of recent trends indicates that CE can show real advantages over chromatographic methods in ultratrace enantioselective determination of biologically active compounds in complex biological matrices. It is due to high separation efficiency and many applicable in-capillary electromigration effects in CE (countercurrent migration, stacking effects) enhancing significantly (enantio)separability and enabling effective sample preparation (preconcentration, purification, analyte derivatization). Other possible on-line combinations of CE, such as column coupled CE-CE techniques and implementation of nonelectrophoretic techniques (extraction, membrane filtration, flow injection) into CE, offer additional approaches for highly effective sample preparation and separation. CE matured to a highly flexible and compatible technique enabling its hyphenation with powerful detection systems allowing extremely sensitive detection (e.g. LIF) and/or structural characterization of analytes (e.g. MS). Within the last decade, more as well as less conventional analytical on-line approaches have been effectively utilized in this field and their practical potentialities are demonstrated on many new application examples in this article. Here, three basic areas of (enantioselective) drug bioanalysis are highlighted and supported by a brief theoretical description of each individual approach in a compact review structure (to create integrated view on the topic), including (i) progressive enantioseparation approaches and new enantioselective agents, (ii) in-capillary sample preparation (preconcentration, purification, derivatization), and (iii) detection possibilities related to enhanced sensitivity and structural characterization.

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Enantioselective analyses of chloroquine and hydroxychloroquine in rat liver microsomes through chiral liquid chromatography–tandem mass spectrometry

Guo

et al. 2021

Chirality

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An efficient, sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) chiral analysis method was established for determination of chloroquine and hydroxychloroquine enantiomers in rat liver microsomes. Effects of polysaccharide chiral stationary phases and basic additives on chiral separations of two analytes were discussed in detail. Amylose tris(3, 5-dimethylphenylcarbamate)-coated chiral stationary phase showed the best separation performance for them with acetonitrile-diethylamine-ethanoldiethylamine mixture (90:0.1:10:0.1, v/v/v/v) among four chiral stationary phases. Then, multiple reaction monitoring mode was selected as the data acquisition for determination of two pairs of enantiomers. The proposed LC-MS/MS chiral analysis method was validated in terms of linearity, accuracy, precision, and specificity. Good linearity with correlation coefficient over 0.998 was obtained in the concentration range of 0.05-5 μM. Limits of quantification for chloroquine and hydroxychloroquine enantiomers were 5.0 and 1.0 nM, respectively. The recoveries ranged from 81.14% to 111.09%. The intra-day and inter-day relative standard deviation were less than 6.5%. Moreover, concentrations of chloroquine and hydroxychloroquine enantiomers in rat liver microsomes were determined through the proposed LC-MS/MS analysis method. After incubated with rat liver microsomes for 10 min, the enantiomeric factor of hydroxychloroquine decreased from 0.50 to 0.45 (p < 0.001). In brief, our developed determination method for chloroquine and hydroxychloroquine enantiomers through LC-MS/MS spectrometry showed the characteristics of high-efficiency, fast speed, and very low detection limit, and would be greatly beneficial for screening and quantitation of them in biological matrices.

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Enantioselective determination of chloroquine and its n‐dealkylated metabolites in plasma using liquid‐phase microextraction and LC‐MS

Cited by 17 publications

References 34 publications

Analytical Methods on Determination in Pharmaceuticals and Biological Materials of Chloroquine as Available for the Treatment of COVID-19

Analytical Methods on Determination in Pharmaceuticals and Biological Materials of Chloroquine as Available for the Treatment of COVID-19

Advanced CE for chiral analysis of drugs, metabolites, and biomarkers in biological samples

Enantioselective analyses of chloroquine and hydroxychloroquine in rat liver microsomes through chiral liquid chromatography–tandem mass spectrometry

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