Search results for "Derivatization"
showing 10 items of 215 documents
Determination of fatty alcohol ethoxylates with diphenic anhydride derivatization and liquid chromatography with spectrophotometric detection
2009
A method for the determination of fatty alcohol ethoxylates (FAEs) using diphenic anhydride as derivatization reagent and RP-HPLC separation with UV-vis detection is presented and compared to derivatization with maleic, phthalic, and other cyclic anhydrides. With these anhydrides, the reaction rates increased when urea was added to the reaction medium, and the yields did not decrease when the samples contained moderate amounts of water. Gradient elution on a C8 column was performed with water/acetonitrile in the presence of 0.1% acetic acid. The use of diphenic anhydride was advantageous for both the chromatographic separation and the detection. Specifically, sensitivity at 200 and 220 nm w…
Selective Derivatization of Calix[4]arenes via Amino Groups Attached to the Wide Rim
2004
A new strategy is proposed for the synthesis of tetraether derivatives of calix[4]arenes bearing at the wide rim nitro and phthalimido groups in well defined positions. Since both groups are precursors of amino functions, calix[4]arenes substituted by different N-acylamino residues are easily available in four steps. The essential steps during the synthesis of the precursor consist in the protection of amino groups by the formation of their phthalimides followed by ipso-nitration of the remaining tert-butylphenol ether units. This nitration occurs without side reactions at the phthalimido substituted units, in contrast to simple N-acyl derivatives.
Determination of tyrosine and phenylalanine by derivatization with nitric acid and differential pulse polarography
1987
Abstract The determination of tyrosine and phenylalanine by differential pulse polarography, after separation by thin-layer chromatography and derivatization with nitric acid to form the nitro compounds, is proposed. Experimental conditions for the derivatization treatment are established and the polarographic determination is optimized.
PEGYLATED POLYASPARTAMIDE–POLYLACTIDE BASED NANOPARTICLES PENETRATING CYSTIC FIBROSIS ARTIFICIAL MUCUS
2016
Here, the preparation of mucus-penetrating nanoparticles for pulmonary administration of ibuprofen in patients with cystic fibrosis is described. A fluorescent derivative of α,β-poly(N-2-hydroxyethyl)-D,L-aspartamide is synthesized by derivatization with rhodamine, polylactide, and poly(ethylene glycol), to obtain polyaspartamide− polylactide derivatives with different degrees of pegylation. Starting from these copolymers, fluorescent nanoparticles with different poly(ethylene glycol) content, empty and loaded with ibuprofen, showed spherical shape, colloidal size, slightly negative ζ potential, and biocompatibility toward human bronchial epithelial cells. The high surface poly(ethylene gly…
BIOADHESIVE PROPERTIES OF A POLYAMINOACIDIC HYDROGEL: EVALUATION BY ATR FT-IR SPECTROSCOPY
2005
The bioadhesive properties of a novel chemical hydrogel based on a polymer of protein-like structure, have been investigated by using ATR FT-IR spectroscopy. In particular, the copolymer PHG obtained by partial derivatization of PHEA with GMA was chemically crosslinked by UV irradiation at 313 nm. Crosslinked PHG was treated with water to obtain a swelled sample, named PHG-UV gel, that was brought into contact with a phosphate buffer/citric acid solution at pH 7.0 in the absence or in the presence of mucin at various concentrations (0.01, 0.1 and 1 wt.-%). Preliminary dynamic swelling studies have evidenced the occurrence of an interaction between the PHG-UV gel and the glycoprotein. This r…
Novel cationic copolymers of a polyasparthylhydrazide: synthesis and characterization.
2005
Alpha,beta-poly(asparthylhydrazide) (PAHy), a water soluble synthetic polymer, was functionalized by using EDCI chemistry with 3-(carboxypropyl)trimethyl-ammonium chloride (CPTACl) obtaining carboxypropyltrimethyl ammonium copolymers (PAHy-CPTA). Three PAHy-CPTA copolymers at increasing derivatization degrees (38%, 48%, 58%) were chosen for subsequent investigations. The capability of these copolymers to bind, neutralize, and protect DNA against degradation by DNase II was evalued by gel retardation assay and DNA degradation test at pH 5.5. Zeta potential measurements show that all studied polymers are able to neutralize the anionic charge of DNA at polymer/DNA weight ratio in the range of …
Fit-for-purpose chromatographic method for the determination of amikacin in human plasma for the dosage control of patients
2015
In this paper, a simple, rapid and sensitive method based on liquid chromatography with fluorimetric detection (HPLC-FLD) for the determination of amikacin (AMK) in human plasma is developed. Determination is performed by pre-column derivatization of AMK with ortho-phtalaldehyde (OPA) in presence of N-acetyl-L-cysteine (NAC) at pH 9.5 for 5 min at 80 °C. In our knowledge, this is the first time that NAC has been used in AMK derivatization. Derivatization conditions (pH, AMK/OPA/NAC molar ratios, temperature and reaction time) are optimized to obtain a single and stable, at room temperature, derivative. Separation of the derivative is achieved on a reversed phase LC column (Kromasil C18, 5 μ…
High-performance micellar liquid chromatography determination of sulphonamides in pharmaceuticals after azodye precolumn derivatization
1995
Abstract A chromatographic procedure with precolumn derivatization to form the N-(1-naphthyl)ethylenediamine dihydrochloride azodyes is proposed for the analysis of several sulphonamides (sodium sulphacetamide, sulphadiazine, sulphaguanidine, sulphamerazine, sulphamethizole, sulphamethoxazole, sulphanilamide and sulphathiazole) in pharmaceutical preparations (tablets, pills, capsules, suspensions and drops). The separation is performed with a 0.05 M sodium dodecyl sulphate/2.4% pentanol eluent at pH 7. The precolumn derivatization improved the resolution in the chromatograms and increased the selectivity in the determination of mixtures of sulphonamides and in preparations where other drugs…
On-line photochemical derivatization and flow-injection spectrophotometric determination of ergonovine maleate
1993
Abstract A flow-injection manifold is proposed for the on-line photochemical derivatization of ergonovine maleate with application to pharmaceutical formulations. The procedure is based on the reaction with p-dimethylaminobenzaldehyde in presence of iron(III) and sulphuric acid medium. The reaction rate is improved by irradiation of the solution with a mercury lamp (254.0 nm). The calibration graph is linear over the range 3–74 μg ml−1 ergonovine, with a mid-range R.S.D. of 1.7% and a sample throughput of 34 h−1. The influence of foreign compounds was tested.
Characterization of the alcoholic fraction of vegetable oils by derivatization with diphenic anhydride followed by high-performance liquid chromatogr…
2008
Abstract Aliphatic and triterpene alcohols present in vegetable oils have been identified and determined by HPLC using UV–vis and MS detection after previous derivatization with diphenic anhydride. The alcoholic fraction was obtained by saponification, extraction and TLC (according to the European Union official procedure). Derivatization was performed in tetrahydrofuran in the presence of suspended grinded urea, which increases the reaction rate and yield. Derivatized extracts were chromatographed on a C8 column using gradient elution with acetonitrile/water mixtures containing 0.1% acetic acid, with UV–vis followed by negative-ion mode MS detection. Using linear discriminant analysis of t…