Simultaneous determination of a hydrophobic drug candidate and its metabolite in human plasma with salting-out assisted liquid/liquid extraction using a mass spectrometry friendly salt

Wu, Huaiqin; Zhang, Jun; Norem, Katherine; El-Shourbagy, Tawakol A.

doi:10.1016/j.jpba.2008.09.002

Cited by 80 publications

(49 citation statements)

References 9 publications

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“…LLE with water-miscible organic solvents had so far been reported for analysis of biological samples [23,24,33]. It can improve the recovery and applicability and greatly reduce the extraction time.…”

Section: Salting Out Assisted Liquid-liquid Extractionmentioning

confidence: 99%

“…3. It has been suggested that NH 4 Ac was a better salting-out agent [24], because of its compatibility with spectrometry. However the recoveries for all the target analytes were very low (<75%), with FB 1 being the least recovered analyte (recovery, <1%).…”

Section: Salting Out Assisted Liquid-liquid Extractionmentioning

confidence: 99%

“…So far, sample preparation using SALLE for multi-mycotoxin analysis from biological fluids has not yet been reported. Most of the applications reported with this method are limited to sample analysis in plasma [22][23][24]. In this paper, we describe the development of a cost-effective, time-efficient and easy-to-use sample preparation method based on SALLE for the simultaneous extraction of the 12 most important mycotoxins and/or their metabolites from pig urine samples.…”

Section: Introductionmentioning

confidence: 99%

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Development and application of salting-out assisted liquid/liquid extraction for multi-mycotoxin biomarkers analysis in pig urine with high performance liquid chromatography/tandem mass spectrometry

Song

Ediage

et al. 2013

Journal of Chromatography A

104

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(2013). Development and application of salting-out assisted liquid/liquid extraction for multi-mycotoxin biomarkers analysis in pig urine with high performance liquid chromatography/tandem mass spectrometry. Journal of Chromatography A, 1292Chromatography A, , 111-120. 10.1016Chromatography A, /j.chroma.2012 AbstractDirect determination of urinary mycotoxins is a better approach to assess individual's exposure than the indirect estimation from average dietary intakes. In this study, a new analytical method was developed and validated for simultaneous analysis of aflatoxin B 1 , deoxynivalenol, fumonisin B 1 , ochratoxin A, zearalenone and T2 toxin and their metabolites in pig urine. In total 12 analytes were selected. A salting-out assisted liquid-liquid extraction procedure was used for sample preparation. High performance liquid chromatography tandem mass spectrometry was used for the separation and detection of all the analytes. The extraction recoveries were in a range of 70% to 108%, with the intra-day relative standard deviation and inter-day relative standard deviation of lower than 25% for most of the compounds at 3 different concentration levels. Meanwhile method bias for all the analytes did not exceed 20%. The method limits of quantification ranged from 0.07 ng mL -1 for ochratoxin A to 3.3 ng mL -1 for deoxynivalenol. Matrix effect was evaluated in this study and matrixmatched calibration was used for quantification. The developed method was also validated for human urine as an extension of its application. Finally, the developed method was applied in a pilot study to analyze 28 pig urine samples. Deoxynivalenol, aflatoxin B 1 , fumonisin B 1 and ochratoxin A were detected in these samples.

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Section: Salting Out Assisted Liquid-liquid Extractionmentioning

confidence: 99%

Section: Salting Out Assisted Liquid-liquid Extractionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Development and application of salting-out assisted liquid/liquid extraction for multi-mycotoxin biomarkers analysis in pig urine with high performance liquid chromatography/tandem mass spectrometry

Song

Ediage

et al. 2013

Journal of Chromatography A

104

View full text Add to dashboard Cite

show abstract

“…Besides widespread conventional and automatic SPE and LLE techniques, newly developed sample preparation techniques including solid phase microextraction [4], liquid-liquid microextraction [5], pressurized liquid extraction [6], molecularly imprinted polymer [7], saltingout liquid-liquid extraction [8], stir bar sorptive extraction [9] and others. Recent investigations have focused on the development of methods to reduce the sample volume required, the analysis time, the cost and the solvent consumption.…”

Section: Introductionmentioning

confidence: 99%

Combination of Extraction by Silylated Vessel-Dispersive Liquid–Liquid Microextraction as a High-Enrichment Factor Technique: Optimization and Application in Preconcentration of Some Triazole Pesticides from Aqueous Samples Followed by GC-FID Determination

et al. 2011

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This study describes an extraction method based on silylated extraction vessel-dispersive liquid-liquid microextraction (SEV-DLLME) for preconcentration of some triazole pesticides (penconazole, hexaconazole, tebuconazole, diniconazole, triticonazole, and difenconazole) from aqueous samples. For this purpose, the interior surface of funnel-shaped extraction vessel is activated by concentrated NaOH and HCl solutions, silylated by trimethylchlorosilane (TMCS) and used in extraction of the analytes from a relatively high volume of aqueous sample. The adsorbed analytes are desorbed by methanol, which acts as a dispersive solvent in the following DLLME method. In the first step, the effects of different factors i.e., concentrations of NaOH, HCl, and silylated agent and their contact times were studied using central composite design (CCD) and response surface method. Extraction time, extraction solvent (chloroform) volume, dispersive solvent (methanol) volume, centrifugation rate and time, and salting-out effect in DLLME procedure were optimized in the same way using CCD, in the second step. High enrichment factors (EFs) (more than 1,000 in most cases) and low detection limits (at sub lg L -1 level) are attainable by using gas chromatography-flame ionization detection. The repeatability and reproducibility of the proposed method are good and the relative standard deviations (RSD %) for six repeated experiments (C = 100 lg L -1 of each pesticide) are less than 7.25%. Finally, the method was successfully applied in determination of analytes in some aqueous samples such as wastewater, well water, and some fruit juice samples.

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“…ISR has gained a lot of momentum in the last few years such that it is now being considered as an integral part of method validation procedure(s), especially when new assays for novel chemical entities (NCEs) and/or important drugs are being developed and marketed (Silvestro et al, 2010;Jemal et al, 2002Jemal et al, , 2010Zhang et al, 2009Zhang et al, , 2010bXu et al, 2009;Fast et al, 2009;Anderson et al, 2009;Myasein et al, 2009;Wu et al, 2008;Huang et al, 2008;Rocci et al, 2007;Larsson and Han, 2007;Brockman et al, 2007). Recently, in a well-compiled report, discussions on the requirements of ISR for macromolecules, with appropriate statistical control, were eloquently presented (Thway et al, 2010).…”

mentioning

confidence: 99%

Incurred sample reanalysis: dilemma in its applicability – should it be practiced for all bioanalytical assays involving single (parent or metabolite) or multiple analytes (parent/metabolite or parent with co‐administered drugs)?

Srinivas¹

2011

Biomedical Chromatography

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Simultaneous determination of a hydrophobic drug candidate and its metabolite in human plasma with salting-out assisted liquid/liquid extraction using a mass spectrometry friendly salt

Cited by 80 publications

References 9 publications

Development and application of salting-out assisted liquid/liquid extraction for multi-mycotoxin biomarkers analysis in pig urine with high performance liquid chromatography/tandem mass spectrometry

Development and application of salting-out assisted liquid/liquid extraction for multi-mycotoxin biomarkers analysis in pig urine with high performance liquid chromatography/tandem mass spectrometry

Combination of Extraction by Silylated Vessel-Dispersive Liquid–Liquid Microextraction as a High-Enrichment Factor Technique: Optimization and Application in Preconcentration of Some Triazole Pesticides from Aqueous Samples Followed by GC-FID Determination

Incurred sample reanalysis: dilemma in its applicability – should it be practiced for all bioanalytical assays involving single (parent or metabolite) or multiple analytes (parent/metabolite or parent with co‐administered drugs)?

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