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Biomedical subjects

V Cavrini

Publications and source records attributed to V Cavrini.

At least 73 records · Page 4Linked to original sources

Analysis of Trimethoprim--sulfonamide drug combinations in dosage forms by UV spectroscopy and liquid chromatography (HPLC).

Derivative and difference spectrophotometric methods are described for the direct simultaneous analysis of combinations of Trimethoprim with sulfonamide drugs (sulfadiazine, sulfamethoxazole, sulfamethoxypyridazine) in commercial dosage forms. The more advantageous approach (derivative and difference mode) is suggested for each binary mixture. The assay results are compared with those obtained by a new chromatographic (HPLC) method, involving a C-18 column and a mobile phase (pH 6.5) containing 1.8 diaminooctane as amine modifier and sodium heptansulfonate as ion pairing agent.

Capsules↗

HPLC study of the impurities present in different ursodeoxycholic acid preparations: comparative evaluation of four detectors.

The use of HPLC with different detectors has been investigated for the analysis of bile acid impurities present in four different commercially available ursodeoxycholic acid preparations. The bile acids were efficiently separated by C18 reversed-phase HPLC using methanol-water (3:2, v/v) as the mobile phase. The detectors used for bile acid detection were: UV at 200 nm refractive index (RI) and an evaporative light scattering mass detector (ELSD II). A prederivatization method with the formation of a fluorescent naphthacyl ester has also been used. GC-MS analysis of Me-TMS bile acid derivatives was included as a reference method. The four ursodeoxycholic acid samples were 98-99% pure. The main impurities present in the samples were chenodeoxycholic acid and to a lesser extent lithocholic acid. Only one sample was found to be almost 100% pure using all the detectors. Significant agreement of the data was found between RI, ELSD II detectors and the fluorescent method; the UV detector was unsuitable for use in this method. The analytical performances of the four detectors for bile acid analysis are reported and discussed. When the four-detector data were compared with the GC-MS method, reasonable agreement resulted. Discordant results were found in the quantitation of trace impurities like lithocholic acid and/or other minor bile acids present in amounts less than 0.1%.

Bile Acids and Salts↗

HPLC-fluorescence determination of bile acids in pharmaceuticals and bile after derivatization with 2-bromoacetyl-6-methoxynaphthalene.

2-Bromoacetyl-6-methoxynaphthalene was used as a pre-chromatographic fluorescent labelling reagent for the high-performance liquid chromatographic (HPLC) analysis of bile acids. The derivatization reaction was performed in an aqueous medium in the presence of tetrahexylammonium bromide by ultrasonication at 40 degrees C to give fluorescent esters which were separated by reversed-phase HPLC and detected fluorimetrically (lambda ex = 300 nm, lambda em = 460 nm). Applications to the determination of ursodeoxycholic acid (UDCA) and chenodeoxycholic acid (CDCA) in their pharmaceutical formulations are described. The method was also applied to the determination of free and conjugated bile acids in human bile samples.

Bile↗

Analysis of flucytosine dosage forms by derivative UV spectroscopy and liquid chromatography.

A simple second-order derivative spectrophotometric method was developed for the selective determination of flucytosine (an antimycotic drug) in the presence of 5-fluorouracil (a cytotoxic agent), its synthetic precursor and degradation product. Traces of 5-fluorouracil in flucytosine were also determined by derivative UV spectroscopy; flucytosine was removed by a selective solid-phase extraction (SPE) procedure using a strong cation-exchange sorbent. The spectrophotometric methods were applied successfully to the quality control of commercial dosage forms of flucytosine and the results were compared with those obtained by a HPLC procedure (cyano column) developed as a reference method.

Chromatography, High Pressure Liquid↗

High-performance liquid chromatographic determination of aliphatic thiols with aroylacrylic acids as fluorogenic precolumn derivatization reagents.

The use of the methyl ester of 4-(6-methoxynaphthalen-2-yl)-4-oxo-2-butenoic acid as a fluorogenic labelling reagent for the high-performance liquid chromatography (HPLC) of biologically important thiols (glutathione, cysteine, acetylcysteine, homocysteine, cysteamine, sodium 2-mercaptoethanesulphonate and thiola) was investigated. The compound reacts selectively and rapidly (10 min at ambient temperature and pH 7.5) with the thiols to give fluorescent adducts that can be separated by reversed-phase HPLC and detected fluorimetrically (lambda em = 450 nm; lambda em = 310 nm). Applications to the determination of L-cysteine and mesna in pharmaceutical formulations are described.

Chromatography, High Pressure Liquid↗

Determination of salicilic acid in saliva by high-performance liquid chromatography.

A sensitive reversed-phase HPLC method with fluorimetric detection was developed for the determination of salicilic acid in saliva samples. The method, involving a preliminary solid-phase extraction procedure, was found to be suitable for the determination of salivary salicilic acid concentrations following the administration of a single oral dose of some commercial acetylsalicilic acid formulations.

Aspirin↗

Determination of minoxidil in pharmaceutical formulations by difference spectrophotometry and liquid chromatography (HPLC).

A simple difference spectrophotometric method has been developed for the selective and rapid determination of minoxidil in pharmaceutical formulations. The method is based on the characteristic modifications of the minoxidil UV spectrum induced by pH changes; a difference spectrum can be obtained and the absorbance A282.8 or the absorbance difference delta A = (A282.8-A259.2) can be used for the selective drug quantitation. As an alternative, a derivative second-order spectrophotometric method was also developed. The spectrophotometric methods were applied to the quality control of commercial minoxidil dosage forms and the results were comparable with those obtained by a reference HPLC procedure.

Chromatography, High Pressure Liquid↗

Analysis of miconazole and econazole in pharmaceutical formulations by derivative UV spectroscopy and liquid chromatography (HPLC).

Methods based on derivative UV spectrophotometry and high-performance liquid chromatography (HPLC) have been developed for the selective determination of miconazole and econazole in pharmaceutical dosage forms. A solid-phase extraction (SPE) procedure using a diol column gave quantitative drug extraction from formulated creams and provided purified sample solutions suitable for assay by the derivative UV spectrophotometric and HPLC methods. The proposed methods gave comparable accurate results, whereas a conventional UV spectrophotometric method was found to be seriously affected by excipients.

Chromatography, High Pressure Liquid↗

Determination of ethacrynic acid in pharmaceutical formulations by difference ultraviolet spectrophotometry after derivatisation with N-acetylcysteine.

A selective difference spectrophotometric procedure is described for the assay of ethacrynic acid (a diuretic drug) in pharmaceutical dosage forms. The method is based on the reaction of the drug with N-acetylcysteine at pH 7.4 and ambient temperature, affording thiol adducts having different spectral properties, and involves the measurement of the absorbance of the reaction mixture relative to an equimolar solution of unreacted ethacrynic acid. The absorbance at 270 nm (A(270)) and the absorbance difference, delta A=A(270-A(244), obtained from the difference spectrum, were found to be linearly correlated with the drug concentration. The proposed spectrophotometric procedure was applied successfully to the determination of ethacrynic acid in pharmaceutical formulations using a reversed-phase high-performance liquid chromatographic procedure as a reference method.

Acetylcysteine↗

Determination of amiodarone hydrochloride in pharmaceutical formulations by derivative UV spectrophotometry and high-performance liquid chromatography (HPLC).

Assay procedures based on derivative ultraviolet spectrophotometry and high-performance liquid chromatography (HPLC) have been developed for the specific determination of amiodarone hydrochloride in pharmaceutical dosage forms. The use of first- and second-order derivative spectrophotometry was found to have suppressed the background absorption from the excipients with comparable accuracy and precision to the reversed-phased HPLC reference method. A conventional UV absorption method (lambda = 242 nm) is subject to possible interference by formulation excipients.

Amiodarone↗

Analysis of nandrolone esters in oily injections by reversed-phase high-performance liquid chromatography.

A specific liquid chromatographic (HPLC) procedure is presented for the analysis of nandrolone esters (phenylpropionate, decanoate and undecanoate) in commercial oily injections. The analysis was carried out under isocratic, reversed-phase (RP8 column) conditions using a UV detector (240 nm). The system discriminates between nandrolone alcohol, a potential impurity, and its esters and permits the quantitation of trace benzaldehyde derived from the oxidative degradation of benzyl alcohol. The proposed HPLC method was found to be more specific and accurate than the pharmacopoeial spectrophotometric assay procedure (isoniazid reagent). The interference of benzaldehyde with the isoniazid method was also investigated.

Journal Article↗