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1.
Anal Chim Acta ; 807: 51-60, 2014 Jan 07.
Article in English | MEDLINE | ID: mdl-24356220

ABSTRACT

Solid-phase microextraction coupled with gas chromatography and mass spectrometry (SPME-GC-MS) was developed for the study of interactions between polycyclic aromatic hydrocarbons (PAHs) and dissolved organic matter (DOM). After the determination of the best conditions of extraction, the tool was applied to spiked water to calculate the dissolved organic carbon water distribution coefficient (K(DOC)) in presence of different mixtures of PAHs and Aldrich humic acid. The use of deuterated naphthalene as internal standard for freely dissolved PAH quantification was shown to provide more accuracy than regular external calibration. For the first time, K(DOC) values of 18 PAHs were calculated using data from SPME-GC-MS and fluorescence quenching; they were in agreement with the results of previous studies. Competition between PAHs, deuterated PAHs and DOM was demonstrated, pointing out the non-linearity of PAH-DOM interactions and the stronger interactions of light molecular weight PAHs (higher K(DOC) values) in absence of high molecular weight PAHs.


Subject(s)
Gas Chromatography-Mass Spectrometry , Polycyclic Aromatic Hydrocarbons/analysis , Solid Phase Microextraction , Water Pollutants, Chemical/analysis , Deuterium/chemistry , Fluorescent Dyes/chemistry , Gas Chromatography-Mass Spectrometry/standards , Humic Substances , Hydrogen-Ion Concentration , Polycyclic Aromatic Hydrocarbons/isolation & purification , Polycyclic Aromatic Hydrocarbons/standards , Reference Standards , Water Pollutants, Chemical/isolation & purification
2.
Pharm Res ; 20(12): 2036-40, 2003 Dec.
Article in English | MEDLINE | ID: mdl-14725371

ABSTRACT

PURPOSE: According to the development in the last decade of industrial processes using high hydrostatic pressure (HHP) for preservation of several commercial food products, novel sterilization or decontamination processes for pharmaceutical products could be conceivable. The aim of this work is to evaluate the effects of HHP on the integrity of insulin and heparin solutions, suspension of monoclonal antibodies and Spherulites. METHODS: High performance liquid chromatography, thin layer chromatography, capillary electrophoresis assays, ELISA tests, laser granulometry and spectrophotometry analyses have been performed to compare HHP treated drugs (in a domain of pressure and temperature ranging respectively from 20 up to 500 MPa and from 20 degrees C up to 37 degrees C) vs. untreated ones. RESULTS: No difference has been detected except for monoclonal antibodies that are altered above 500 MPa. CONCLUSIONS: The structure integrity of sensitive molecule due to the small energy involved by HHP and the development of industrial plants (intended for the decontamination of food products) confer to this technology the potential of a new method for sterilization of fragile drugs and an original alternative to aseptic processes and sterilizing filtration.


Subject(s)
Drug Delivery Systems , Pharmaceutical Preparations/chemistry , Antibodies, Monoclonal/administration & dosage , Antibodies, Monoclonal/chemistry , Chromatography, High Pressure Liquid , Chromatography, Thin Layer , Drug Compounding , Electrophoresis, Capillary , Enzyme-Linked Immunosorbent Assay , Hardness , Heparin/administration & dosage , Heparin/chemistry , Hydrostatic Pressure , Insulin/administration & dosage , Insulin/chemistry , Particle Size , Peptides/chemistry , Solutions , Suspensions , Temperature
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