Basic Sample Preparation Techniques in LC‐MS Bioanalysis

Li, Wenkui; Jian, Wenying; Fu, Yunlin

doi:10.1002/9781119274315.ch1

Cited by 18 publications

(31 citation statements)

References 63 publications

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“…They proposed the Twister Back-Extraction (TBE) procedure: it takes place putting the stir bar and the sample into a vial. The bar stirs the sample solution until the concentration of the target analytes in the sample reaches the equilibrium with that in the PDMS coating [48], thus it is a non-exhaustive technique. After extraction, the operator cleans the stir bar and puts it into a clean vial where the desorption of the target compounds with a proper solvent takes place.…”

Section: Twister Back-extraction Tbementioning

confidence: 99%

“…After extraction, the operator cleans the stir bar and puts it into a clean vial where the desorption of the target compounds with a proper solvent takes place. After the back extraction, the solvent containing the target compounds is injected in interfaced instruments with appropriate detection modes TBE is the most efficient way of using the SBSE applied to liquid chromatography and high performance liquid chromatography [48]. The principles of this technique are the same as SPME with PDMS-coated fibers, but the volume of the extraction phase is 50-250 times more massive [49].…”

Section: Twister Back-extraction Tbementioning

confidence: 99%

“…Monolithic columns are one piece of silica rod or organic polymer with flow-through pores. The smaller pores entail large surface areas for sufficient separation capacity, while the larger ones reduce flow resistance [48]. These materials overcome problems of large void volume between the packed particles and slow mass transfer, typical in conventional particulate material [82].…”

Section: On-linementioning

confidence: 99%

“…These materials have a pore size that provides size exclusion and hydrophilic shielding preventing large molecules from entering the inner region of the sorbent. At the same time, the porosity is such that lets the small molecule analytes access the internal region of the sorbent, where retention takes place [48]. Accordingly, only small molecules can penetrate the pores and interact with a RAM stationary phase.…”

Section: On-linementioning

confidence: 99%

“…Immobilized antibodies onto a pressureresistant support make a material that can fit into an extraction column. They can remove a specific analyte from complex matrices affording high selectivity and sensitivity [48].…”

Section: On-linementioning

confidence: 99%

See 4 more Smart Citations

A review of micro-solid-phase extraction techniques and devices applied in sample pretreatment coupled with chromatographic analysis

Dugheri

Marrubini

Mucci

et al. 2021

Acta Chromatographica

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Sample pretreatment is one of the most crucial and error-prone steps of an analytical procedure; it consents to improve selectivity and sensitivity by sample clean-up and pre-concentration. Nowadays, the arousing interest in greener and sustainable analytical chemistry has increased the development of microextraction techniques as alternative sample preparation procedures. In this review, we aimed to show two different categorizations of the most used micro-solid-phase extraction (μSPE) techniques. In essence, the first one concerns the solid-phase extraction (SPE) sorbent selection and structure: normal-phase, reversed-phase, ion-exchange, mixed-mode, molecular imprinted polymer, and special techniques (e.g., doped cartridges for specific analytes). The second is a grouping of the commercially available μSPE products in categories and sub-categories. We present every device and technology into the classifications paying attention to their historical development and the actual state of the art. So, this study aims to provide the state-of-the-art of μSPE techniques, highlighting their advantages, disadvantages, and possible future developments in sample pretreatment.

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Section: Twister Back-extraction Tbementioning

confidence: 99%

Section: Twister Back-extraction Tbementioning

confidence: 99%

Section: On-linementioning

confidence: 99%

Section: On-linementioning

confidence: 99%

Section: On-linementioning

confidence: 99%

See 3 more Smart Citations

A review of micro-solid-phase extraction techniques and devices applied in sample pretreatment coupled with chromatographic analysis

Dugheri

Marrubini

Mucci

et al. 2021

Acta Chromatographica

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Toxicokinetics in preclinical drug development of small‐molecule new chemical entities

Picard

2022

Biomedical Chromatography

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Toxicokinetics (TK) is an integral part of nonclinical (preclinical) safety assessment of small-molecule new chemical entities in drug development. It is employed to describe the systemic exposure of a drug candidate and/or its important metabolite(s) achieved in study animals and elucidate the relationship (proportional, over-proportional, or under-proportional) between systemic exposure and dose administered and the associated differences/similarities between male and female animals along with the possible accumulation/induction. TK data and the derived parameters are employed to propose safe starting doses for clinical use of the new drug candidate through proper extrapolation of findings in study animals to humans. This review has attempted to highlight the health authority expectations on TK assessment in supporting preclinical safety profiling of new chemical entities. A robust TK assessment requires good understanding of absorption, distribution, metabolism, and elimination processes of drug candidate, adequate TK sampling (e.g., controls where relevant), implementation of fit-for-purpose bioanalytical methods (validated or scientifically qualified) along with necessary measures to prevent mis-dosing or ex vivo contamination, and establishment of stability of the drug candidate and/or its metabolite(s) in the intended species matrix to ensure the reliability of bioanalytical and TK data. The latter provides a vital link between animal experiments and human safety.

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LC–MS/MS bioanalytical method for the quantitative analysis of nifedipine, bisoprolol, and captopril in human plasma: Application to pharmacokinetic studies

Abdel‐Megied

Kovalenko

Elbarbry

et al. 2023

Biomedical Chromatography

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In this study, the development and validation of an accurate and highly sensitive LC–MS/MS method were performed for the estimation of nifedipine, bisoprolol and captopril in real human plasma. Liquid–liquid extraction using tert‐butyl methyl ether was efficiently applied for extraction of the analytes from plasma samples. The chromatographic separation was carried out using an isocratic elution mode on the X‐terra MS C18 column (4.6 × 50 mm, 3.5 μm). The mobile phase consisted of methanol–0.1% formic acid (95:5, v/v) for determination of nifedipine and bisoprolol and acetonitrile–0.1% formic acid (70:30, v/v) for determination of captopril with a flow rate of 0.5 ml/min. Acceptable results regarding the different validation characteristics of the analytes were obtained in accordance with US Food and Drug Administration recommendations for bioanalytical methods. The developed approach was linear over concentration ranges of 0.5–130.0, 50.0–4,500.0 and 0.3–30.0 ng/ml for nifedipine, captopril and bisoprolol, respectively. The method revealed a sufficient lower limit of quantification in the range of 0.3–50.0 ng/ml, as well as high recovery percentages, indicating high bioanalytical applicability. The proposed method was efficiently applied to a pharmacokinetic evaluation of a fixed‐dose combination of the analytes in healthy male volunteers.

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Basic Sample Preparation Techniques in LC‐MS Bioanalysis

Cited by 18 publications

References 63 publications

A review of micro-solid-phase extraction techniques and devices applied in sample pretreatment coupled with chromatographic analysis

A review of micro-solid-phase extraction techniques and devices applied in sample pretreatment coupled with chromatographic analysis

Toxicokinetics in preclinical drug development of small‐molecule new chemical entities

LC–MS/MS bioanalytical method for the quantitative analysis of nifedipine, bisoprolol, and captopril in human plasma: Application to pharmacokinetic studies

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