Microextraction sample preparation techniques in biomedical analysis.

Biologically active compounds are found in biological samples at relatively low concentration levels. The sample preparation of target compounds from biological, pharmaceutical, environmental, and food matrices is one of the most time-consuming steps in the analytical procedure. The microextraction techniques are dominant.

Identification of In Vitro Metabolites of Amoxicillin in Human Liver Microsomes by LC-ESI/MS.

Amoxicillin (AMOX) metabolism in human liver microsomes was studied in vitro using liquid chromatography-mass spectrometry (LC/MS). Amoxicillin was incubated with human liver microsomes along with NADPH, and the reaction mixture was analyzed by LC/MS to obtain the specific metabolic profile of the studied antibiotic drug. Positive electrospray ionization was employed as the ionization source.

Determination of ascorbic acid and its degradation products by high-performance liquid chromatography-triple quadrupole mass spectrometry.

This study describes application of liquid chromatography coupled with triple quadrupole mass spectrometry (LC-MS) for evaluation of vitamin C stability, the objective being prediction of the degradation products. Detection was performed with an UV detector (UV-Vis) in sequence with a triple-quad mass spectrometer in the multiple reaction mode. The negative ion mode of ESI and MS-MRM transitions of m/z 175→115 (quantifier) and 175→89 (qualifier) for ascorbic acid was used.

Simultaneous determination of selected chemotherapeutics in human whole blood by molecularly imprinted polymers coated solid phase microextraction fibers and liquid chromatography-tandem mass spectrometry.

Development and validation of novel, general liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the simultaneous determination of amoxicillin (AMOX), cefatoxime (CEF), ciprofloxacin (CIP), daptomycin (DAPTO), fluconazole (FLU), gentamicin (GEN), clindamycin (KLI), linezolid (LIN), metronidazole (MET), moxifloxacin (MOXI) in human whole blood are described. Samples were prepared on solid phase microextraction way with the use of polymeric sorption coatings with molecular imprints and analyzed using a gradient separation over an ACE C18-column (4.6mm×150mm, 3μm) with isocratic elution.

Pharmacokinetic study of amoxicillin in human plasma by solid-phase microextraction followed by high-performance liquid chromatography-triple quadrupole mass spectrometry.

Sensitive and selective analytical procedures based on high-performance liquid chromatography with mass spectrometric detection were developed for the determination of amoxicillin in human plasma samples. Samples were prepared by applying in-house manufactured molecularly imprinted solid-phase microextraction probes. The detection of target compounds was performed in multiple reaction monitoring mode.

A new approach for antibiotic drugs determination in human plasma by liquid chromatography-mass spectrometry.

Sensitive and selective analytical procedures based on high performance liquid chromatography with mass spectrometric detection were developed for the determination of linezolid (LIN) and amoxicillin (AMOX) in human plasma samples. Samples were prepared by applying protein precipitation (PP), solid phase extraction (SPE), and microextraction in packed syringe (MEPS). The analytical separation was carried out using reversed phase liquid chromatography in isocratic mode.

New approaches to extraction techniques in determination of 4,4'-methylenebis(2-chloroaniline) in air and water solutions.

Extraction techniques for 4,4'-methylenebis(2-chloroaniline) (MOCA) in air samples and water solutions were developed and compared. Classic techniques for air sampling of MOCA were enhanced by incorporating a derivatization step (3,5-dinitrobenzoyl chloride solution in toluene), thus increasing the limit of detection and limit of quantification. Sampling of MOCA from water solution was performed using novel nanoporous polymeric (polypyrrole and polythiophene) fiber coatings and solid phase microextraction.

Development of novel molecularly imprinted solid-phase microextraction fibers and their application for the determination of antibiotic drugs in biological samples by SPME-LC/MS(n).

Novel molecularly imprinted polymer (MIP)-coated fibers for solid-phase microextraction (SPME) fibers were prepared by using linezolid as the template molecule. The characteristics and application of these fibers were investigated. The polypyrrole, polythiophene, and poly(3-methylthiophene) coatings were prepared in the electrochemical polymerization way.

A new way of solid-phase microextraction fibers preparation for selected antibiotic drug determination by HPLC-MS.

The polypyrrole (PPy) and polythiophene (PTh) solid phase microextraction (SPME) coatings were obtained with the use of the electropolymerisation and linear sweep voltammetry. Such fibers were modified by an ozone treatment in a gaseous phase in the concentration of 2.1 ± 0.

Poly(3-alkylthiophenes): new sorption materials for solid phase microextraction of drugs isolated from human plasma.

A novel sorbent in solid phase microextraction (SPME) method based on poly(3-alkylthiophenes) was used in the isolation of linezolid from human plasma samples following liquid chromatography determination. The effect of extraction time on the sorption capacity of the SPME process was studied and pointed at 10 min both for adsorption and desorption. Poly(3-methylthiophene) and poly(3-nonylthiophene) were applied for the extraction of linezolid from water solutions.

A novel approach to the rapid determination of amoxicillin in human plasma by solid phase microextraction and liquid chromatography.

A new approach to the rapid determination of amoxicillin (AMO) in human plasma followed by solid phase microextraction (SPME) fiber coatings based on conducting polymers (polypyrrole and polythiophene) and high performance liquid chromatography (HPLC) has been described. The porous structures of the electrochemically deposited polymer coatings have been characterized by scanning electron microscopy (SEM). The experimental parameters relating to the extraction efficiency of the SPME fibers such as pH, extraction time and desorption conditions (solvents, time) were studied and selected.

New coated SPME fibers for extraction and fast HPLC determination of selected drugs in human blood.

Polythiophene (PTh) and polypyrrole (PPy) as sorbent phases for solid phase microextraction (SPME) were applied in order to extract the multi-resistant Staphylococcus aureus (MRSA) antibiotic drugs (linezolid and daptomycin) from whole blood followed by high performance liquid chromatography (HPLC) determination with UV detection. Relative standard deviations (RSDs) of in vitro and pseudo in vivo measurements performed in whole blood were in the range of 4.58-15.

Fibers with polypyrrole and polythiophene phases for isolation and determination of adrenolytic drugs from human plasma by SPME-HPLC.

In this study, polypyrrole (PPy) and polythiophene (PTh) SPME coatings and their ability to extract selected adrenolytic drugs with different physico-chemical properties from standard solutions and human plasma samples were evaluated. In measurements metoprolol, oxprenolol, mexiletine, propranolol, and propaphenon were investigated. The main parameters such as extraction time, desorption conditions and pH influence were examined.

Polypyrrole solid phase microextraction: A new approach to rapid sample preparation for the monitoring of antibiotic drugs.

Simple or even rapid bioanalytical methods are rare, since they generally involve complicated, time-consuming sample preparation from the biological matrices like LLE or SPE. SPME provides a promising approach to overcome these limitations. The full potential of this innovative technique for medical diagnostics, pharmacotherapy or biochemistry has not been tapped yet.

Determination of adrenolytic drugs by SPME-LC-MS.

Five adrenolytic drugs have been analyzed by liquid chromatography-mass spectrometry (LC-MS). Samples were prepared by solid-phase microextraction (SPME) using polypyrrole fibers coated on stainless steel support as an adsorbent for the drugs. Adsorption efficiencies were 95% and were close for all the drugs investigated.