Microextraction in a Packed Syringe for the Analysis of Olive Biophenols in Rat Plasma Using CMK-3 Nanoporous Sorbent

Abstract

A carbon-based nanoporous sorbent was first used for microextraction in a packed syringe (MEPS) before HPLC/UV analysis of some biophenols in rat plasma. A laboratory-made programmable apparatus was designed and used for automation of the extraction procedure. The MEPS syringe was packed with 2 mg of CMK-3 sorbent, between the barrel and the injection needle, and mounted on an apparatus for programming of the conditioning, sampling, washing, elution and cleaning steps. All steps of the microextraction procedure were carefully optimized on the system. For optimization of important factors, such as the number of adsorption and elution cycles, elution volume and pH, a multivariate central composite design method was used. The highest recoveries were obtained for 24 and 10 times of adsorption and elution cycles, respectively, using 100 μL of acetonitrile as the eluent and a sample pH of 2. Good results were obtained in terms of the precision (RSD 1.6, 2.5 and 2.3%) and detection limit (0.7, 4.7 and 0.25 μM) for caffeic acid, tyrsol and oleuropein, respectively. The method was simple, efficient and appropriate for sample clean up before analysis by HPLC, and was successfully applied to the determination of biophenols in the plasma of several rats that received an olive leaves extract either by a gavage or an intraperitoneal injection method. A positive correlation was found between the amount of olive extract's feeding of the rats and the level of their plasma biophenols.

Nanostructured star‐shaped polythiophene dendrimer as a highly efficient sorbent for microextraction in packed syringe for HPLC analysis of the Clofentezine in milk and juice samples

“…In this method, only 1–2 mg of sorbent is used which can handle sample volumes from 10 to 1000 μL. the sorbent material is inserted into the barrel of a syringe as a plug with filters on both sides, or between the syringe barrel and the injection needle . The sample is withdrawn several times through the packed bed inside the syringe barrel, so that the analyte adsorbs on the solid‐phase sorbent.…”

Current trends on microextraction by packed sorbent – fundamentals, application fields, innovative improvements and future applications

“…This has been elegantly used to find the presence of olive biophenols, caffeic acid, oleuropein and tyrsol, in rat plasma following the ingestion of olive oil. 149 To perform this assay the authors developed a new MEPS sorbent, a carbon nanoporous adsorbent (CMK-3), and the extraction was followed by a LC-UV analysis. A similar assay was performed Legend: *elution solvent composition is indicated in v/v ratios and these are discriminated only when they are not equivalent among the components of the mixtures used; Au/LDHpacked hybrids of gold nanoparticles and layered double hydroxide nanosheets; DADdiode array detector; FLDfluorescence detection; HDVBhighly crosslinked polystyrene divinylbenzene; HPLChigh performance liquid chromatography; LODslimits of detection; LOQslimits of quantification; M1mixed-mode C8/SCX MEPS sorbent; MEPSmicroextraction by packed sorbent; MSmass spectrometry; MS/MStandem MS; MIL-101(Cr)metal-organic framework (MOF)-based catalyst, chromium hydroxide number 101; PDAphotodiode array detector; PEPpolar enhanced polymer MEPS sorbent; PGCporous graphitic carbon MEPS sorbent; R(A/C)Xpolymeric DVB partially functionalized with quaternary amine groups or sulfonic acid groups, respectively; SAXstrong anion exchange; SCXstrong cation exchange; Silsilica MEPS sorbent; SVOCssemi-VOCs; VSMC/CMCvascular smooth muscle cells/cell membrane chromatography; UHPLCultra high performance liquid chromatography; UVultraviolet detection; µECDmicroelectron-capture detector.…”

Paradigm Shift in the Arena of Sample Preparation and Bioanalytical Approaches Involving Liquid Chromatography Mass Spectroscopic Technique

“…MEPS is an upgraded version over SPE towards a more efficient and sophisticated format that reduces the volumes of sample, washing and elution solvent. 125 MEPS resemble a miniaturized SPE packed bed device with a different range of volumes. In MEPS, the sample extraction, concentration, and clean-up steps are performed in a single device composed of a syringe and a MEPS barrel insert and needle (BIN).…”