Determination of several psychiatric drugs in whole blood using capillary gas–liquid chromatography with nitrogen phosphorus detection: comparison of two solid phase extraction procedures

Torre, Carolina Sánchez de la; Martínez, María Antonia; Almarza, Elena

doi:10.1016/j.forsciint.2004.12.007

Cited by 80 publications

(36 citation statements)

References 24 publications

(36 reference statements)

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“…Moreover and above all, OCLLE provides the real advantage over LLE to avoid emulsion formation in ensuring immiscibility of organic solvents and aqueous matrix. This, therefore, significantly eases extraction procedure [23]. Fidente et al [24] have developed an extraction procedure based on identical principles for insecticide analysis in honey, but this study involved a single class of insecticides and therefore included a limited number of chemically related compounds.…”

Section: Extraction Assaysmentioning

confidence: 99%

Development and validation of a multi-residue method for pesticide determination in honey using on-column liquid–liquid extraction and liquid chromatography–tandem mass spectrometry

Pirard

Widart

Nguyen

et al. 2007

Journal of Chromatography A

109

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We report on the development and validation under ISO 17025 criteria of a multi-residue confirmatory method to identify and quantify 17 widely chemically different pesticides (insecticides: Carbofuran, Methiocarb, Pirimicarb, Dimethoate, Fipronil, Imidacloprid; herbicides: Amidosulfuron, Rimsulfuron, Atrazine, Simazine, Chloroturon, Linuron, Isoxaflutole, Metosulam; fungicides: Diethofencarb) and 2 metabolites (Methiocarb sulfoxide and 2-Hydroxytertbutylazine) in honey. This method is based on an on-column liquid-liquid extraction (OCLLE) using diatomaceous earth as inert solid support and liquid chromatography (LC) coupled to mass spectrometry (MS) operating in tandem mode (MS/MS). Method specificity is ensured by checking retention time and theoretical ratio between two transitions from a single precursor ion. Linearity is demonstrated all along the range of concentration that was investigated, from 0.1 to 20 ngg -1 raw honey, with correlation coefficients ranging from 0.921 to 0.999, depending on chemicals. Recovery rates obtained on home-made quality control samples are between 71 and 90%, well above the range defined by the EC/657/2002 document, but in the range we had fixed to ensure proper quantification, as levels found in real samples could not be corrected for recovery rates. Reproducibility is found to be between 8 and 27%. Calculated CCα and CCβ (0.0002-0.943 ngg -1 for CCα, and 0.0002-1.232 ngg -1 for CCβ) show the good sensitivity attained by this multi-residue analytical method. The robustness of the method has been tested in analyzing more than 100 raw honey samples collected from different areas in Belgium, as well as some wax and bee samples, with a slightly adapted procedure.

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Section: Extraction Assaysmentioning

confidence: 99%

Development and validation of a multi-residue method for pesticide determination in honey using on-column liquid–liquid extraction and liquid chromatography–tandem mass spectrometry

Pirard

Widart

Nguyen

et al. 2007

Journal of Chromatography A

109

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“…Ces techniques sont employées dans les domaines de l'environnement pour la recherche de pesticides [15,21,22], de l'agroalimentaire [21], de la pharmacocinétique avec le dosage de médicaments comme le clopidogrel et son métabolite [23], de la médecine du travail [24] ou en toxicologie par le screening de benzodiazépines [25] ou encore la recherche d'antidé-presseurs [26,27]. La comparaison des rendements d'extraction de benzodiazépines par cette technique (60 à 90 %) ne montre pas d'infériorité par rapport à la technique classique (80 à 90 %) [25].…”

Section: Extraction Liquide-liquide Sur Support Solideunclassified

Extraction liquide-liquide : théorie, applications, difficultés

2010

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Résumé -Les méthodes d'extraction liquide-liquide (ELL) permettent le transfert d'un soluté initialement contenu dans une phase liquide vers une autre phase liquide non miscible. Elles sont couramment employées en pharmacologie/toxicologie afin de purifier et concentrer les échantillons préalablement à une analyse par méthode chromatographique. Divers paramètres physico-chimiques régissent la réalisation d'une ELL, propres aux solvants employés et aux solutés à extraire. La connaissance de certaines propriétés du solvant telles sa miscibilité à l'eau, sa constante d'acidité, sa constante diélectrique, son moment dipolaire, sa densité, sa volatilité ainsi que sa toxicité permettront le choix de ce solvant seul ou en mélange pour l'extraction d'une substance donnée. De la même manière, la connaissance des propriétés du soluté telles sa structure, sa constante d'acidité, sa lipophilie, la nature et la complexité de la matrice dans laquelle il se trouve, permettront d'optimiser l'extraction, dont l'efficacité sera évaluée par le rendement d'extraction. L'influence de ces paramètres sera abordée dans cette revue, et les différents processus d'ELL (extraction simple, multiple, back-extraction, formation de paires d'ions) seront exposés simultanément avec leurs avantages et inconvénients respectifs. La maîtrise de toutes ces variables permettra à l'opérateur une optimisation des étapes d'ELL lors de la mise au point de méthodes d'analyse en pharmacologie/toxicologie. Mots clés : Extraction liquide-liquide, solvants, soluté, propriétés physico-chimiquesAbstract -Liquid-liquid extraction (LLE) methods allow transfer of compounds solubilized in a liquid phase into another immiscible liquid phase. These methods are routinely used in pharmacology/toxicology so as to purify and concentrate biological samples before chromatographic analysis. Many different physico-chemical properties of solvents and solutes have to be taken into account in LLE. To perform an extraction, the choice of a solvent or of a mixture of solvents depends on their miscibility with water, proticity, dielectric constant, dipole moment, density, volatility and toxicity. In the same way, the evaluation of properties of solutes such as structure, acidity constant and lipophily, together with the nature and complexity of the matrix, will allow the optimization of the extraction process. Its efficiency will be evaluated with the extraction recovery. The influence of these parameters will be discussed in this review, and the different extraction processes (single, multiple, back-extraction and ion-pair formation) will be described with their respective advantages and drawbacks. The control of all these variables should allow the operator to optimize LLE during development of analytical methods in pharmacology/toxicology.

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“…Sometimes a poorly adapted dosing of these drugs can worsen the patient status due to their eventual toxicity and this is particularly the case for tricyclic antidepressants, barbiturates and first generation antipsychotics. Moreover, due to their widespread use, psychotropic drugs are frequently involved in cases of deliberate and accidental poisoning (Sanchez De La Torre, Martinez, & Almarza, 2005;Smink et al, 2004). So far in Rwanda, the determination of BCLs of these drugs is not done regardless of the case.…”

Section: Introductionmentioning

confidence: 99%

Transfer of high performance liquid chromatography with diode array detection method for determination in serum of psychotropic drugs

Hahirwa

Charlier

Karangwa

et al. 2017

RWJour

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Background: The relevance of the determination of blood concentration levels of psychotropic drugs has been demonstrated in Rwanda. However, due to the lack of appropriate analytical methods, such activity is not carried out in this country. Objective: The aim of this work was to transfer to a Rwandan laboratory a High Performance Liquid Chromatography based method, applicable for the determination in serum of psychotropic drugs commonly prescribed in Rwanda. Method: Liquid-liquid extraction using prazepam as internal standard was used for sample preparation. Chromatographic separation was performed on a Symmetry C8 analytical column, using acetonitrile and a phosphate buffer as mobile phase. The method was validated with respect to total error concept as decision criterion. Results: The validated method was linear over tested dosing intervals with a coefficient of determination greater than 0.99 for all analytes. The precision was good with RSD between 1.3 and 15.6% and the trueness ranged between 87 and 109%.The accuracy of the method was demonstrated as well. Conclusion: The analytical method allowing a simultaneous determination in serum of several antipsychotropic drugs was successfully validated and thus transferred to the Laboratory of Analysis of Foodstuffs, Drugs, Water and Toxics (Rwanda).

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Determination of several psychiatric drugs in whole blood using capillary gas–liquid chromatography with nitrogen phosphorus detection: comparison of two solid phase extraction procedures

Cited by 80 publications

References 24 publications

Development and validation of a multi-residue method for pesticide determination in honey using on-column liquid–liquid extraction and liquid chromatography–tandem mass spectrometry

Development and validation of a multi-residue method for pesticide determination in honey using on-column liquid–liquid extraction and liquid chromatography–tandem mass spectrometry

Extraction liquide-liquide : théorie, applications, difficultés

Transfer of high performance liquid chromatography with diode array detection method for determination in serum of psychotropic drugs

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