Overcoming non-specific adsorption issues for AZD9164 in human urine samples: Consideration of bioanalytical and metabolite identification procedures

Silvester, Steve; Zang, Frank

doi:10.1016/j.jchromb.2012.03.004

Cited by 22 publications

(14 citation statements)

References 18 publications

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“…Recently, similar problems regarding adsorption losses have been reported for the analysis of quaternary drugs from urine samples 10,12 . Urine matrix is similar in constituents to environmental aqueous samples.…”

Section: Introductionmentioning

confidence: 69%

Micelle Assisted Thin-Film Solid Phase Microextraction: A New Approach for Determination of Quaternary Ammonium Compounds in Environmental Samples

Boyacı

Pawliszyn

2014

Anal. Chem.

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Keywords: High throughput analysis, Quaternary ammonium compounds, Sample preparation of challenging compounds, Thin-film solid phase microextraction, Micelle-modified matrix, micelleassisted stabilization of quaternary ammonium compounds, micelle assisted TF-SPME 2 ABSTRACTDetermination of quaternary ammonium compounds (QACs) often is considered to be a challenging undertaking owing to secondary interactions of the analytes' permanently charged quaternary ammonium head or hydrophobic tail with the utilized lab-wares.Here, for the first time, a micelle assisted thin-film solid phase microextraction (TF-SPME) using a zwitterionic detergent 3-[(3-cholamidopropyl)dimethylammonio]-1-propanesulfonate (CHAPS) as a matrix modifier is introduced as a novel approach for in-laboratory sample preparation of the challenging compounds.The proposed micelle assisted thin-film solid phase microextraction (TF-SPME) method offers suppression/enhancement free electrospray ionization of analytes in mass spectrometric detection, minimal interaction of the micelles with the TF-SPME coating, and chromatographic stationary phase and analysis free of secondary interactions. Moreover, it was found that the matrix modifier has multiple functions; when its concentration is found below the critical micelle concentration (CMC), the matrix modifier primarily act as a surface deactivator; above its CMC, it acts as a stabilizer for QACs. Additionally, shorter equilibrium extraction times in the presence of the modifier demonstrated that micelles also assist in the transfer of analytes from the bulk of the sample to the surface of the coating.The developed micelle assisted TF-SPME protocol using the 96-blade system requires only 30 min of extraction and 15 min of desorption. Together with a conditioning step (15 min), the entire method is 60 min; considering the advantage of using the 96-blade system, if all the blades in the brush are used, the sample preparation time per sample is 0.63 min. Moreover, the recoveries for all analytes with the developed method were found to range within 80.2%-97.3%; as such, this 3 method can be considered an open bed solid phase extraction. The proposed method was successfully validated using real samples.4

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Section: Introductionmentioning

confidence: 69%

Micelle Assisted Thin-Film Solid Phase Microextraction: A New Approach for Determination of Quaternary Ammonium Compounds in Environmental Samples

Boyacı

Pawliszyn

2014

Anal. Chem.

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“…The adsorption of analytes on container material is an occasionally observed issue also described for analytical studies dealing with urine samples (Heinig, Wirz, Yuan, Tingler, & Mylott, ; Ji et al, ; Li, Luo, Smith, & Tse, ). Interestingly, in a publication by Silvester and Zang (), adsorption of a test compound (AZD9164, ( R )‐1‐(4‐fluorophenethyl)‐3‐{[( S )‐2‐phenyl‐2‐(piperidin‐1‐yl)propanoyl]oxy}quinuclidin‐1‐ium), which shares some structural features with D‐84, toward plastic material of containers in urine samples, is reported. Several types of additives (such as proteins, detergents or cosolvents) are known to overcome this problem.…”

Section: Resultsmentioning

confidence: 99%

“…Several types of additives (such as proteins, detergents or cosolvents) are known to overcome this problem. Owing to concerns that addition of proteins may lead to undesired interferences in the binding experiments and addition of detergents may cause severe matrix problems in LC‐ESI‐MS/MS‐based marker quantification, we decided to make use of dimethylacetamide (DMA), which has already been reported to prevent adsorption of AZD9164 in urine samples in the above‐mentioned study (Silvester & Zang, ). For investigation of the effect of DMA on the adsorption of rac ‐D‐84 ( rac ‐ 1 ) to the container, dilution series at six concentration levels between 500 p m and 25 n m were prepared in water without and with the addition of DMA and analyzed concerning their relative response factors (see Supporting Information).…”

Section: Resultsmentioning

confidence: 99%

Development and validation of an LC‐ESI‐MS/MS method for the quantification of D‐84, reboxetine and citalopram for their use in MS Binding Assays addressing the monoamine transporters hDAT, hSERT and hNET

Neiens

Simone

Ramershoven

et al. 2018

Biomedical Chromatography

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MS Binding Assays represent a label-free alternative to radioligand binding assays. In this study, we present an LC-ESI-MS/MS method for the quantification of (R,R)-4-(2-benzhydryloxyethyl)-1-(4-fluorobenzyl)piperidin-3-ol [(R,R)-D-84, (R,R)-1], (S,S)-reboxetine [(S,S)-2], and (S)-citalopram [(S)-3] employed as highly selective nonlabeled reporter ligands in MS Binding Assays addressing the dopamine [DAT, (R,R)-D-84], norepinephrine [NET, (S,S)-reboxetine] and serotonin transporter [SERT, (S)-citalopram], respectively. The developed LC-ESI-MS/MS method uses a pentafluorphenyl stationary phase in combination with a mobile phase composed of acetonitrile and ammonium formate buffer for chromatography and a triple quadrupole mass spectrometer in the multiple reaction monitoring mode for mass spectrometric detection. Quantification is based on deuterated derivatives of all three analytes serving as internal standards. The established LC-ESI-MS/MS method enables fast, robust, selective and highly sensitive quantification of all three reporter ligands in a single chromatographic run. The method was validated according to the Center for Drug Evaluation and Research (CDER) guideline for bioanalytical method validation regarding selectivity, accuracy, precision, calibration curve and sensitivity. Finally, filtration-based MS Binding Assays were performed for all three monoamine transporters based on this LC-ESI-MS/MS quantification method as read out. The affinities determined in saturation experiments for (R,R)-D-84 toward hDAT, for (S,S)-reboxetine toward hNET, and for (S)-citalopram toward hSERT, respectively, were in good accordance with results from literature, clearly demonstrating that the established MS Binding Assays have the potential to be an efficient alternative to radioligand binding assays widely used for this purpose so far.

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“…Additives investigated for reducing non-specific binding include the addition of albumin (Carneheim and Stahle, 1991), beta-cyclodextrin (Khramov and Stenken, 1999a), CHAPS [(3-cholamidopropyl) dimethylammonio-1-propanesulphonate] (Silvester and Zang, 2012) or polysorbate-80 (Loos et al, 2007) in order to saturate the binding sites on the microdialysis tubing and dialysis membrane (Pitt et al, 1988;Traunmuller et al, 2006), thereby reducing the non-specific binding of compounds. In our experiments, compounds tested exhibited varying degrees of non-specific binding to the test system.…”

Section: Discussionmentioning

confidence: 99%

Approach to reduce the non-specific binding in microdialysis

Nirogi

Kandikere

Bhyrapuneni

et al. 2012

Journal of Neuroscience Methods

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Overcoming non-specific adsorption issues for AZD9164 in human urine samples: Consideration of bioanalytical and metabolite identification procedures

Cited by 22 publications

References 18 publications

Micelle Assisted Thin-Film Solid Phase Microextraction: A New Approach for Determination of Quaternary Ammonium Compounds in Environmental Samples

Micelle Assisted Thin-Film Solid Phase Microextraction: A New Approach for Determination of Quaternary Ammonium Compounds in Environmental Samples

Development and validation of an LC‐ESI‐MS/MS method for the quantification of D‐84, reboxetine and citalopram for their use in MS Binding Assays addressing the monoamine transporters hDAT, hSERT and hNET

Approach to reduce the non-specific binding in microdialysis

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