HPLC-fluorescence determination of chlorocresol and chloroxylenol in pharmaceuticals.

The use of 2-chloro-6,7-dimethoxy-3-quinolinecarboxaldehyde as a fluorogenic labelling reagent in pre-column derivatization for the HPLC separation of chlorophenols has been investigated. The compound reacts (50 min at 110 degrees C) with 2- and 4-chlorophenols to give fluorescent ethers that can be separated by reversed-phase HPLC and detected at lambda exc = 360 nm, lambda em = 500 nm. The experimental conditions for derivatization and chromatographic separation are discussed. Applications for the determination of chlorocresol (4-chloro-3-cresol) and chloroxylenol (4-chloro-3,5-xylenol) in pharmaceutical formulations (creams, ointments) are described.

GC-MS analysis of incenses for possible presence of allergenic nitromusks.

A Gas chromatographic method with mass detector was developed to identify and determine nitromusks in incense sticks of different origin (India, China, Tibet). The proposed method was found useful to correlate dermatological allergic reactions with the use and composition of commercial incense sticks. The incense sticks were powdered, extracted with methanol and after the addition of 1-eicosanol as internal standard, injected into the GC-MS, using 25 m bonded phase fused capillary column methyl, 5% phenyl silicone (0.32 mm I.D., 0.25 microns film thickness). Musk ambrette was identified and determined in one kind of chinese incense together with musk ketone and musk xylene. The latter compound was also found alone in another kind of chinese incense.

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.

[Synthesis of various acyclic analogs of pyrimidine nucleosides]. / Sintesi di alcuni analoghi aciclici di nucleosidi pirimidinici.

As acyclic analogues of pyrimidine nucleosides, 1-[2-(2,3- dihydroxypropyloxy )ethyl]pyrimidines (III a-c) and 1-[[3-(2,3- dihydroxypropyloxy )-2-hydroxy]propyl]pyrimidines (III d-f) were synthesized and tested for in vitro activity against herpes simplex virus type 1. The compounds exhibited no significant antiherpetic activity.

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.

[Effect on lipidemia in the rat of bis-homoanalogs of adenine nucleosides]. / Azioni sulla lipidemia del ratto di bis-omoanaloghi di nucleosidi dell'adenina.

The hypolipidemic activity of a series of adenine nucleosides bis-homoanalogues was evaluated in the rat and compared with that of the sodium salt of erythadenine, used as reference standard. Some compounds were more effective in lowering serum cholesterol than erythadenine, but all showed a reduced effect on serum triglyceride content.

Antiviral compounds. XVII - Synthesis and in vitro antiviral activity of 1-substituted 2-chloro- and 2-methoxyindole-3-carboxaldehyde thiosemicarbazones.

A series of indole-3-carboxaldehyde thiosemicarbazones with substituent variations at the 1 and 2 positions were prepared and evaluated for in vitro antiviral activity against vaccinia virus strain IHD and parainfluenza virus type 3, HA-I/CR-8 strain. The inhibitory activity of most compounds was restricted to the vaccinia virus, only compounds (III e) and (III f) being effective against both viruses. Structure-activity relationship are discussed.

[Synthesis and in vitro antibacterial activity of N-methylnitrone and nitrovinyl derivatives of some N-substituted 2-chloroindol-3-carboxaldehydes]. / Sintesi ed attività antibatterica in vitro di N-metilnitroni e nitrovinili derivati da alcune 2-cloroindol-3-carbossialdeidi N-sostituite.

N-methylnitrones and nitrovinyl derivatives from 1-substituted-2-chloroindol-3-carboxaldehydes were synthesized and evaluated for their in vitro antibacterial activity. Some nitrovinyl derivatives displayed good in vitro activity against Gram-positive bacteria; the compound (II e), 1-(o-chlorobenzyl)-2-chloro-3-(2-nitroethenyl)indole, was more active than nitrofurantoin against Staphylococcus aureus and Streptococcus pyogenes. Some structure-activity relationships are discussed.

[Synthesis of 2-methoxynaphthalene derivatives as potential anti-inflammatory agents]. / Sintesi di derivati della 2-metossinaftalina come potenziali antiinfiammatori.

Compounds having 2-methoxynaphthalene as their parent nucleus were synthesized and evaluated for antiinflammatory effect according to the carrageenin paw edema method in rats. The synthetic routes for the preparation of isomeric 1,2- and 2,6-disubstituted derivatives are described. Replacement of the alpha-methylacetic moiety in naproxen by 4-hydroxybutyric acid side chain did not cause loss of activity.

[Substances with antiviral activity. XV. Preparation and antiherpes activity of alkyl- and acylamino-dihalogenated pyrimidines and pyridines]. / Ricerche su sostanze ad attività antivirale. Nota XV - Preparazione e attività antierpetica di alchil- e acilammino- -dialogeno-pirimide e -piridine.

Some dihalo-amino-pyrimidines and -pyridines were alkylated and acylated at the amino group. The resulting twenty-four compounds were then tested for their action on Herpes simplex virus infection in human HEp-2 cell cultures. Five compounds were active and 2-benzamido-3,5-dichloropyridine [(III B); Table I] showed the highest antiviral activity.