Morphine and its metabolites: Analytical methodologies for its determination

Bosch, M. Espinosa; Sánchez, Ángel Galán; Rojas, F. Sánchez; Ojeda, C. Bosch

doi:10.1016/j.jpba.2006.12.005

Cited by 54 publications

(26 citation statements)

References 163 publications

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“…During the first set of 11 experiments used for chemometric optimization (2 3 FFL DoE, Table 1 The second part of the ZIC-HILIC method development was focused on the differences between the alkaloid polarities, the amphoteric properties of some of MO, CO and OR as well as the limited water solubility of NS and PV. The chromatographic behaviour of analytes was investigated at different mobile phase pH values (3)(4)(5)(6)(7)(8) to obtain a pH profile for components in the mixture. This was determined by two independent 2 2 CCC DoEs with basic and acidic mobile phases (Equation 2), where each set included 11 planned experiments (Table 2) investigating pH (x 1 ) (3.0-5.0 for the acidic profile and 6.0-8.0 for the basic profile) and ionic strength of the mobile phase buffer (x 2 ) (10-100 mM ammonium formate buffer for the acidic profile and 10-100 mM ammonium ace-tate for the basic profile).…”

Section: Development and Optimization Of The Zic-hilic Methodsmentioning

confidence: 99%

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Chemometric approach for development, optimization and validation of HILIC methods used for the determination of alkaloids from poppy straw

Acevska

Stefkov

Nakov

et al. 2014

Maced. J. Chem. Chem. Eng.

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Two hydrophilic interaction liquid chromatography (HILIC) methods for simultaneous determination of the major alkaloids (morphine, codeine, thebaine, oripavine, papaverine and noscapine) present in opium poppy straw (Papaver somniferum L., Papaveraceae) were developed. The chromatographic behavior of the target alkaloids was investigated on two different HILIC stationary phases (bare silica, Si-HILIC; zwitterionic, ZIC-HILIC) and systematic optimization carried out using chemometrics. A full factorial design of the experiments was utilized to assess the influence of acetonitrile content, ionic strength and pH of the mobile phase buffer on the critical resolutions and relevant retention factors. Central composite circumscribed design of experiments was used for robustness testing during method validation. The separation of alkaloids was obtained within a close retention window on both columns with optimized gradient elution, though the ZIC-HILIC method had advantages over Si-HILIC method in terms of sensitivity, robustness and cost. This method was found suitable for the determination of the morphinan alkaloids in poppy straw.Keywords: chemometry; design of experiments; HILIC/DAD; opium poppy alkaloids ХЕМОМЕТРИСКИ ПРИСТАП ЗА РАЗВОЈ, ОПТИМИЗАЦИЈА И ВАЛИДАЦИЈА НА HILIC-МЕТОДИ ЗА ОПРЕДЕЛУВАЊЕ АЛКАЛОИДИ ОД АФИОНОВИ ЧУШКИРазвиени се две методи за едновремено определување на главните алкалоиди (морфин, кодеин, тебаин, орипавин, папаверин и носкапин) од афион (Papaver somniferum L., Papaveraceae) со примена на течна хроматографија со хидрофилна интеракција (HILIC).Хроматографското однесување на целните алкалоиди е испитувано на две различни стационарни фази за течна хроматографија со хидрофилна интеракција: необработена силика (Si-HILIC) и цвитерјонска стационарна фаза (ZIC-HILIC).Влијанието на хроматографските фактори (содржина на ацетонитрил, јонска јачина и рН-вредност на пуферот во составот на мобилната фаза) врз неколку хроматографски параметри е проценето со примена на факторски дизајн на експериментите. Квадратен модел од трет ред (Central Composite Circumscribed Design of Experiments) е користен за утврдување на робусноста во рамките на валидацијата на методите.Разделувањето на алкалоидите е постигнато во двете колони со оптимизирано градиентно елуирање. Методот ZIC-HILIC има предност пред методот Si-HILIC во однос на сензитивност, ро-бусност и цена. Овој метод е погоден за определување на морфинските алкалоиди од афионови чушки.Kлучни зборови: хемометрија; дизајн на експерименти; HILIC/DAD; опиумски алкалоиди од афион

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Section: Development and Optimization Of The Zic-hilic Methodsmentioning

confidence: 99%

“…High performance liquid chromatography (HPLC) is an efficient technique for the separation and quantification of opium alkaloids [2][3][4][5][6][7][8][9][10][11]. Due to the large polarity range of the major opium alkaloids, most applications use RP-HPLC with gradient elution and ion-pairing agents.…”

Section: Introductionmentioning

confidence: 99%

Chemometric approach for development, optimization and validation of HILIC methods used for the determination of alkaloids from poppy straw

Acevska

Stefkov

Nakov

et al. 2014

Maced. J. Chem. Chem. Eng.

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“…HPLC-MS/MS is the method of choice for simultaneous analysis of morphine and M6G in human serum reviewed by Bosch et al [6] and was used for this setting. Our investigations were intended to provide a robust and validated, according to Food and Drug Administration (FDA) guidelines [7], HPLC-MS/MS protocol for determination of morphine and M6G in human plasma and give example for clinical use in intensive care patients.…”

Section: Introductionmentioning

confidence: 99%

HPLC-MS/MS Based Time Course Analysis of Morphine and Morphine-6- Glucoronide in ICU Patients

Andreas¹,

Peter²,

Lerch³

et al. 2017

J Chromatogr Sep Tech

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“…En effet, seule la morphine libre est dosée par cette méthode : une seconde analyse, réalisée après une étape d'hydrolyse acide ou enzymatique, est nécessaire pour déterminer la morphine totale et permettre de déduire la concentration des métabolites glucuronoconjugués totaux de la morphine [8,9]. Compte tenu du faible volume attendu des prélèvements sanguins chez le lapin, une méthode de dosage simultané de la morphine et de ses métabolites glucuronoconjugués totaux par chromatographie liquide à haute performance couplée à la spectrométrie de masse (LC-MS) a été dévelop-pée.…”

Section: Introductionunclassified

Mise au point et validation d’une méthode de dosage simultané de la morphine et de ses métabolites glucuronoconjugués totaux par chromatographie liquide d’interactions hydrophiles

et al. 2010

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Résumé -Objectif : Dans le cadre d'une étude expérimentale de redistribution post-mortem des xénobiotiques menée chez le lapin, une méthode de dosage simultané de la morphine et de ses métabolites glucuronoconjugués totaux dans des échantillons de sang total de faible volume a été développée. Méthode : Les étalons internes deutérés sont ajoutés à une prise d'essai de 100 μL. La préparation des échantillons consiste en l'extraction liquide-solide sur des cartouches Oasis r HLB (Waters r , Saint-Quentin-en-Yvelines, France). L'analyse est menée par chromatographie liquide haute performance couplée à la spectrométrie de masse en mode d'ionisation électrospray. Les composés d'intérêt sont élués par chromatographie liquide d'interactions hydrophiles au travers d'une colonne Luna r HILIC -150 mm × 2,0 mm × 3 μm (Phenomenex r , Le Pecq, France). La méthode de dosage est validée selon le concept de l'erreur totale à l'aide du logiciel e-noval r (Chemcad, Obernai, France). Résultats : Les fonctions de réponse sont de type quadratique non pondéré. Les résultats sont linéaires sur l'ensemble de l'intervalle de dosage des analytes soit de 10 à 300 ng/mL pour la morphine et de 750 à 10 000 ng/mL pour ses métabolites glucuronoconjugués totaux. La limite de détection estimée est de 3,5 ng/mL pour la morphine et de 250 ng/mL pour ses métabolites glucuronoconjugués totaux. Les incertitudes de mesure sont respectivement de 15 % et de 9 %. Conclusion : L'extraction liquide-solide sur cartouches Oasis r HLB et la chromatographie liquide d'interactions hydrophiles, adaptées à la séparation des molécules polaires, ont permis de mettre au point une méthode de dosage simultané de la morphine et de ses métabolites glucuronoconjugués totaux sur de faibles volumes d'échantillons. Mots clés : Morphine, métabolites glucuronoconjugués, chromatographie liquide haute pression, chromatographie liquide d'interactions hydrophilesAbstract -Aim: As part of an experimental post-mortem drugs' redistribution study in rabbits, a method for simultaneous determination of morphine and total morphine glucuronides in small volume whole blood samples was developed. Method: The deuterated internal standards are added to a sample of 100 μL. Sample preparation is performed by solidphase extraction on Oasis r HLB cartridges (Waters r , Saint-Quentin-en-Yvelines, France). The analysis is carried out by high performance liquid chromatography -electrospray ionization mass spectrometry. The separation of analytes is obtained by hydrophilic interaction liquid chromatography with a Luna r HILIC column -150 mm × 2.0 mm × 3 μm (Phenomenex r , Le Pecq, France). Analytical method is validated according to the total error approach with e-noval r software (Chemcad, Obernai, France). Results: Response functions are unweighted quadratic regressions. Analytical method is linear in measuring intervals: from 10 to 300 ng/mL for morphine and 750 to 10 000 ng/mL for total morphine glucuronides. The estimated detection limit is 3.5 ng/mL for morphine and 250 ng/mL for total morphin...

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Morphine and its metabolites: Analytical methodologies for its determination

Cited by 54 publications

References 163 publications

Chemometric approach for development, optimization and validation of HILIC methods used for the determination of alkaloids from poppy straw

Chemometric approach for development, optimization and validation of HILIC methods used for the determination of alkaloids from poppy straw

HPLC-MS/MS Based Time Course Analysis of Morphine and Morphine-6- Glucoronide in ICU Patients

Mise au point et validation d’une méthode de dosage simultané de la morphine et de ses métabolites glucuronoconjugués totaux par chromatographie liquide d’interactions hydrophiles

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