Development of a UHPLC-MS/MS method for the determination of 84 pharmaceuticals and drugs of abuse in human liver

Orfanidis, Amvrosios; Gika, Helen; Theodoridis, Georgios; Mastrogianni, Orthodoxia; Raikos, Νikolaos

doi:10.1016/j.jchromb.2020.122192

Cited by 19 publications

(9 citation statements)

References 15 publications

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“…The first one is made of 1.6 µm solid-core particles, while the second one is made of 1.7 µm porous particles having a bridged ethyl-siloxane silica hybrid (BEH) structure. Both are expected to improve resolution and efficiency of separation and have been successfully used for determination of pharmaceuticals (except sotalol) in water matrices [17,27,34,35]. These columns were assessed with a gradient elution 0.1% ammonium formate (AF) used as aqueous eluent, while 0.1% to 0.3% AF in ACN were tested as organic eluents, based on the assumption that shifting pH to acid will serve a better separation of targeted molecules.…”

Section: Methods Developmentmentioning

confidence: 99%

“…As can be seen from the physical-chemical properties of these four molecules, their simultaneous determination may be challenging since these compounds present a wide range of properties such as polarity, solubility, acid dissociation constants, partition coefficients, and stabilities under acidic and basic conditions [25]. Even if ultra-high pressure liquid chromatography (UHPLC) and tandem mass spectroscopy (MS n ) using updated source designs and acquisition methods is known to allow detection of pharmaceuticals at very low concentrations, especially by use of smaller particle size chromatographic columns (below 2.0 µm) [25][26][27], simultaneous determination of such compounds within the same chromatographic method has not been yet reported, even in papers dealing with multi-residue analysis of pharmaceuticals. Indeed, sotalol (hydrophilic and polar) is often better detected by use of an hydrophilic column [28], whereas fluoxetine and azithromycin (lipophilic and moderately polar) and erythromycin (lipophilic and non-polar) are separated by reversed-phase C18 [26,27,29,30].…”

Section: Introductionmentioning

confidence: 99%

“…Even if ultra-high pressure liquid chromatography (UHPLC) and tandem mass spectroscopy (MS n ) using updated source designs and acquisition methods is known to allow detection of pharmaceuticals at very low concentrations, especially by use of smaller particle size chromatographic columns (below 2.0 µm) [25][26][27], simultaneous determination of such compounds within the same chromatographic method has not been yet reported, even in papers dealing with multi-residue analysis of pharmaceuticals. Indeed, sotalol (hydrophilic and polar) is often better detected by use of an hydrophilic column [28], whereas fluoxetine and azithromycin (lipophilic and moderately polar) and erythromycin (lipophilic and non-polar) are separated by reversed-phase C18 [26,27,29,30]. In the present study, we developed a UHPLC-MS method using a novel column stationary phase capable of providing a selectivity within a wide elution window and increased retention for both polar and non-polar analytes.…”

Section: Introductionmentioning

confidence: 99%

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Fast UHPLC-MS/MS for the Simultaneous Determination of Azithromycin, Erythromycin, Fluoxetine and Sotalol in Surface Water Samples

et al. 2021

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Chromatographic development for the determination of pharmaceuticals in environmental water samples is particularly challenging when the analytes have significantly different physico-chemical properties (solubility, polarity, pKa) often requiring multiple chromatographic methods for each active component. This paper presents a method for the simultaneous determination of azithromycin, erythromycin (antibiotics), fluoxetine (anti-depressant) and sotalol (b-blocker) in surface waters by ultra-high-performance liquid chromatography coupled with ultra-high-resolution time-of-flight mass spectrometry. These pharmaceuticals—presenting a broad spectrum of polarity (0.24 ≤ log Kow ≤ 4.05)—were separated on a C-18 analytical column, after a simple filtration step for freshwater samples or after a liquid–liquid extraction with Methyl-tertio-butyl ether (MTBE) for seawater samples. The optimized separation method (in terms of nature of column and eluent, elution gradient, and of mass spectrometric parameters), enable one to reach limits of detection ranging between 2 and 7 ng L−1 and limits of quantification between 7 and 23 ng L−1 for the four targeted molecules, within a three minute run. This method was validated using samples collected from three different surface waters in Lebanon (freshwater and seawater) and analytical results were compared with those obtained in surface waters sampled in a French river, equivalent in terms of human activities. Using this method, we report the highest concentration of pharmaceuticals found in surface water (up to 377 ng L−1 and 268 ng L−1, respectively, for azithromycin and erythromycin, in the Litani river, Lebanon).

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Section: Methods Developmentmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Fast UHPLC-MS/MS for the Simultaneous Determination of Azithromycin, Erythromycin, Fluoxetine and Sotalol in Surface Water Samples

et al. 2021

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“…This method is a modification of the QuEChERS (quick, easy, cheap, effective, rugged and safe) initially introduced for the extraction of pesticides in fruit and vegetable by Anastassiades et al. [8] , which has been subjected to several modification to improve the overall technique performance in other matrices and analytes [9] , [10] , [11] , [12] , [13] , [14] , [15] . The compounds extracted and analyzed in soil with the QuEChERS-based method constitute a large group of 305 organic compounds.…”

Section: Introductionmentioning

confidence: 99%

Extension of an extraction method for the determination of 305 organic compounds in clay-loam soil to soils of different characteristics

et al. 2021

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Highlights These results allowed to broaden the range of soils that can be analyzed with the proposed methodology. In the worst case (loamy sand soil), the original methodology allowed the analysis of 180 compounds with adequate recoveries. For analytes outside the acceptable range in this soil and the other soil type analyzed, correction factors are proposed.

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“…ples and organic solvents, which has led to its use in different matrices and analytes [38]. Modified versions of QuEChERS have been successfully applied in soils for the extraction of organic contaminants, including pesticides [39][40][41], persistent organic pollutants [42,43], as well as in the extraction of ARs and PhACs from other samples such as food [44,45], blood [46,47], sediments and sludge [48], and the liver [49,50].…”

Section: Introductionmentioning

confidence: 99%

An Easy Procedure to Quantify Anticoagulant Rodenticides and Pharmaceutical Active Compounds in Soils

Acosta-Dacal

Rial-Berriel

Díaz-Díaz

et al. 2021

Toxics

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A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction was validated for the extraction of seven coumarin anticoagulant rodenticides (ARs) and 36 pharmaceutical active compounds (PhACs) residues in soil samples using liquid chromatography tandem mass spectrometry (LC-MS/MS). The aim of this work was to develop a method for the monitoring of these compounds in agricultural lands as well as in forensic applications for the determination of ARs poisoning. As far as is known, this is the first time that a QuEChERS-based method is used for the extraction of ARs in soil, as well as on such a quantity of PhACs. A matrix effect study was carried out on samples of soil devoted to agriculture in the midland area of the Canary Islands (clay loam type). It was in house validated (accuracy, precision, and linearity) at seven spiked levels between 0.5 and 50 ng g−1. The limits of quantification (LOQ) ranged between 0.5 and 50.0 ng g−1 and the limits of detection (LOD) ranged from 0.024 to 6.25 ng g−1. The method was then successfully used for both the determination of the target analytes in the soils from the agricultural plots that had been irrigated with regenerated water, and in the soil collected from underneath wild bird carcasses (which had been the subject of forensic investigation).

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Development of a UHPLC-MS/MS method for the determination of 84 pharmaceuticals and drugs of abuse in human liver

Cited by 19 publications

References 15 publications

Fast UHPLC-MS/MS for the Simultaneous Determination of Azithromycin, Erythromycin, Fluoxetine and Sotalol in Surface Water Samples

Fast UHPLC-MS/MS for the Simultaneous Determination of Azithromycin, Erythromycin, Fluoxetine and Sotalol in Surface Water Samples

Extension of an extraction method for the determination of 305 organic compounds in clay-loam soil to soils of different characteristics

An Easy Procedure to Quantify Anticoagulant Rodenticides and Pharmaceutical Active Compounds in Soils

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