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At least 757 records · Page 42Linked to original sources
PubMed1998

Automated on-line dialysis for sample preparation and HPLC analysis of antidepressant drugs in human plasma. Inhibition of interaction with the dialysis membrane.

Antidepressant drugs interact with the dialysis membrane and were selected as model substances to study inhibition of analyte-membrane interactions. A chemometric approach based on response surface modelling was used for screening and optimisation of dialysis recoveries. Optimal dialysis recoveries (52-65%) were obtained for the model compounds (mianserine, amitriptyline, nortriptyline, imipramine and desimipramine) when a cationic surfactant added to the donor solution of the dialyser was used to inhibit analyte-membrane interactions. Automated analysis of antidepressants in plasma was performed by connecting the ASTED (Automated Sequential Trace Enrichment of Dialysates) system to high-performance liquid chromatography (HPLC). The drugs were detected by ultraviolet detection and fluorescence detection after post-column photochemical reaction. Validation of the method showed linear standard curves for all the drugs in the concentration range 50-2000 nmol 1-1. Within-and between day relative standard deviations ranged from 1.1 to 5.7%.

Antidepressive Agents↗
PubMed2002

Evaluation of sample preparation techniques for mass measurements of PCR products using ESI-FT-ICR mass spectrometry.

Elimination of PCR buffer components and alkali metal cations (i.e., Na+, K+) is of critical importance to allow for accurate mass measurements of PCR products for genotyping and sequencing applications. Ethanol precipitation followed by microdialysis has been repeatedly shown to efficiently desalt PCR products for analysis by mass spectrometry and is considered the gold standard. Alternative cleanup techniques that are compatible with automation are explored here with the intent of expanding the bottleneck that exists between the production of PCR products and analysis by electrospray ionization mass spectrometry (ESI-MS). Numerous combinations of approaches were evaluated that included PCR purification kits and alcohol precipitations. The data shown here support alternative approaches to an ethanol precipitation followed by microdialysis that have comparable desalting efficiency and can be utilized for cleanup of PCR products generated from single reactions.

2-Propanol↗
PubMed2003

Quantitative determination of benazepril and benazeprilat in human plasma by gas chromatography-mass spectrometry using automated 96-well disk plate solid-phase extraction for sample preparation.

An analytical method for the determination of benazepril and its active metabolite, benazeprilat, in human plasma by capillary gas chromatography-mass-selective detection, with their respective labelled internal standard, was developed and validated according to international regulatory requirements. After addition of the internal standards, the compounds were extracted from plasma by solid-phase extraction using automated 96-well plate technology. After elution, the compounds were converted into their methyl ester derivatives by means of a safe and stable diazomethane derivative. The methyl ester derivatives were determined by gas chromatography using a mass-selective detector at m/z 365 for benazepril and benazeprilat and m/z 370 for the internal standards. Intra- and inter-day accuracy and precision were found to be suitable over the range of concentrations between 2.50 and 1000 ng/mL.

Benzazepines↗
PubMed1992

Combined supercritical fluid extraction/solid-phase extraction with octadecylsilane cartridges as a sample preparation technique for the ultratrace analysis of a drug metabolite in plasma.

Supercritical fluid extraction was coupled with solid-phase extraction using octadecylsilane cartridges for the selective isolation of ultratrace levels of a drug metabolite, mebeverine alcohol, from plasma. Plasma was directly applied to the extraction cartridge, the cartridge was washed to remove protein and then extracted under supercritical conditions using CO2/5% methanol. The effluent from the extraction cell was bubbled through a small volume of 2-propanol to trap the extracted mebeverine alcohol. The effects of extraction pressure and temperature on analyte recovery were examined. The absolute recovery, selectivity, precision, and accuracy of the combined supercritical fluid extraction/solid-phase extraction approach were compared to those of conventional solid-phase extraction using gas chromatography/mass spectrometry in the selected-ion monitoring mode. Mebeverine alcohol was used as a model compound, and dog plasma was employed as the biological matrix for these studies.

Animals↗
PubMed2006

Deamidation of -Asn-Gly- sequences during sample preparation for proteomics: Consequences for MALDI and HPLC-MALDI analysis.

We find that peptides containing -Asn-Gly- sequences typically show approximately 70-80% degree of deamidation after standard overnight (approximately 12 h) tryptic digestion at 37 degrees C. This emphasizes the need for more detailed information about the deamidation reaction in -Asn-Gly- sequences, in which two deamidated species are produced, one containing an aspartic acid (-Asp-Gly-) residue and the other containing an isoaspartic acid (-betaAsp-Gly-) residue. For the peptide SLNGEWR (54-60 beta-galactosidase, E. coli), all three components of the reaction mixture were separated by HPLC on C18 300-A sorbent, with trifluoroacetic acid as an ion-pairing modifier. Their intensity ratios suggested the elution order -betaAsp-/-Asn-/-Asp-, which was subsequently confirmed by MALDI MS and MS/MS analysis. The kinetics of the deamidation was studied in detail for the synthetic SLNGEWR parent using RP HPLC with UV detection. The half-life of this peptide was found to be approximately 8 h under digestion conditions. Analysis of a large pool of peptide retention data shows that the -betaAsp-/-Asn-/ -Asp- retention order is normally observed under the above conditions, especially if the original -NG- sequence is surrounded by hydrophobic amino acids. However, changing chromatographic conditions to 100-A pore size sorbents, or using formic acid as a modifier, increases the retention time of -betaAsp- relative to the -Asn-/-Asp- pair, so the order can sometimes be different.

Amides↗
PubMed2003

Sample preparation and presampling of pistachios.

A theory has been developed to quantify the reduction of subsample variance of aflatoxin contamination, which is observed when granular materials are wet slurried, rather than dry ground, during subsample homogenization. A coefficient of variation, based on particle size distribution, subsample size, and probability of contamination, is predicted. The theory is tested with dry ground and with wet slurried pistachios, and excellent quantitative agreement is obtained. A 32% increase in the mean aflatoxin level is observed as well when wet slurrying is applied. Although no statistical explanation for this effect can be found, it is suggested that it is related to physiochemical binding between the nut matrix, which is (partly) broken by wet slurrying, and aflatoxin, making the extraction of more toxin possible. Other parameters that may affect slurrying results have been investigated as well.

Aflatoxins↗
PubMed1988

Biological sample preparation and data reduction concepts in pharmaceutical analysis.

This paper describes strategies to rapidly develop sensitive and selective preparations using manual and robotic liquid-solid isolation (LSI) methods. LSI procedures offer selective isolation of drug or metabolites from complex matrices and are applicable to many pharmaceutical compounds. The beneficial effect of weighted linear regression is described, and several data reduction techniques are contrasted.

Chemical Phenomena↗