Use of fouling resistant nanofiltration and reverse osmosis membranes for dyeing wastewater effluent treatment.

Dyeing wastewater was post-treated by using nanofiltration (NF) and reverse osmosis (RO) membranes. To reduce membrane fouling, poly (vinyl alcohol) (PVA) with a neutral charge was coated on NF and RO membranes. The effect of surface charge and surface roughness on membrane fouling was investigated. Dyeing wastewater was pre-treated by using coagulation, activated sludge process, and MF process to investigate the effect of the pre-treatment on the membrane fouling. It is demonstrated that the extent of fouling is significantly influenced by the surface roughness and the surface charge on the NF and RO membranes. A membrane with a smooth and neutral surface was fouled less. The pre-treatment was essential for avoiding NF and RO membranes fouling. The quality of the final permeate was acceptable for water reuse.

Metabolism of dimethyl-4,4'-dimethoxy-5,6,5',6'-dimethylene dioxybiphenyl-2,2'-dicarboxylate (DDB) by human liver microsomes: characterization of metabolic pathways and of cytochrome P450 isoforms involved.

Metabolic fate of DDB and identification of P450 isozymes involved in the metabolism of DDB were investigated in human liver microsomes. DDB was rapidly metabolized to five different metabolites, and the structures of each metabolite were characterized based on UV, mass, and NMR spectral analyses. The major metabolic pathways of DDB in human liver microsomes were identified as O-demethylation of the carboxymethyl moiety (M4) and demethylenation of the methylenedioxyphenyl group (M2). The intramolecular lactonization between the hydroxyl group at the C6 and carboxymethyl group at the C2' of M2 resulted in the generation of M5, which was either hydrolyzed to its hydrolyzed derivative (M1) or further metabolized to the O-demethylated derivative (M3). The interconversion of M1, M2, and M5 took place nonenzymatically depending on the solvent condition. M5 was predominantly detected at the acidic condition, whereas M1 was preferentially detected at the basic environment. Cytochrome P450 (P450) isoform(s) involved in the metabolism of DDB was identified using several in vitro approaches. Chemical inhibition using isoform-selective P450 inhibitors, correlation of DDB metabolites formation with several isoform-specific P450 activities in a panel of liver microsomes, metabolism by microsomes derived from P450 cDNA-expressed B-lymphoblastoid cells, and immunoinhibition by isoform-specific anti-P450 antibodies collectively indicated that CYP1A2, CYP2C9, and CYP3A4 are responsible for the metabolism of DDB. O-Dealkylation of the carboxymethyl group was preferentially catalyzed by CYP1A2, whereas demethylenation of the methylenedioxyphenyl moiety was catalyzed by CYP3A4 and CYP2C9.

Characterization of amiodarone metabolites and impurities using liquid chromatography/atmospheric pressure chemical ionization mass spectrometry.

Using the high performance liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry (HPLC/APCI-MS/MS) technique, together with established trends from the literature, the structures of metabolites and impurities of amiodarone, an anti-arrhythmic drug, have been assigned. By comparing analyses of products of incubation with rat liver microsomes with controls in which glucose 6-phosphate dehydrogenase was omitted, metabolites could be distinguished from impurities. Structures for the two proposed metabolites and four impurities are proposed.

In vitro inducible nitric oxide synthesis inhibitors from Alismatis Rhizoma.

Bioassay-guided fractionation of an aqueous extract of Alismatis Rhizoma has furnished two inducible nitric oxide synthase (iNOS) inhibitory compounds, alismol (1) and alisol B monoacetate (2), together with an inactive triterpene, alisol C monoacetate (3). Compounds 1 and 2 inhibited nitric oxide (NO) synthesis in a dose-dependent manner in murine macrophage-like RAW 264.7 cells stimulated with interferon-gamma (IFN-gamma) plus lipopolysaccharide (LPS). The inhibitory effects of 1 and 2 on NO synthesis were partly due to suppression of iNOS mRNA expression as determined by Northern blotting.

Determination of homocysteine and its related compounds by solid-phase microextraction-gas chromatography-mass spectrometry.

The purpose of this study was to develop a simple and accurate analytical method to determine homocysteine (Hcy), cysteine (Cys), and methionine (Met) in aqueous samples. Until now, the most frequently used method for the assay of Hcy, Cys, and Met has been high-performance liquid chromatography with fluorescence detection after fluorescent tagging. The newly developed method involves the employment of the SPME (solid-phase microextraction) technique together with GC-MS. For application to a gas chromatographic system, alkyl formate derivatives were prepared in the form of N(O,S)-alkoxycarbonyl alkyl ester with the analytes in the aqueous samples. The optimum derivatizing regent for N(O,S)-alkoxycarbonyl alkyl ester was chosen by comparing the efficiency of the derivatized analytes in a GC through the SPME method and liquid-liquid extraction. The optimum conditions of the SPME system for the analytes derivatized with N(O,S)-ethoxycarbonyl propyl ester in the aqueous matrix were pH 3.0 and no salt, and 30 min equilibration time using an 85 microm PA (polyacrylate) fiber. The developed method is inexpensive, easy and rapid.

Identification of IY81149 and its metabolites in the rat plasma using the on-line HPLC/ESI mass spectrometry.

Reversed-phase high-performance liquid chromatography/mass spectrometry (HPLC/MS) with an electrospray ionization (ESI) interface was applied to the identification of metabolites of IY 81149 in the rat plasma. Fragments obtained using collision-induced dissociation (CID) in both positive and negative modes were utilized to elucidate the structure of metabolites. The eluent from the conventional HPLC column was split and directly introduced into an ESI-mass spectrometer for the identification of the structures. The CID technique allowed the sensitive identification of sulfonyl-IY81149 and hydroxy-IY81149 from the rat plasma.

Solid-phase microextraction for the determination of pethidine and methadone in human urine using gas chromatography with nitrogen-phosphorus detection.

A simple and rapid analytical method is presented for the determination of pethidine (meperidine) and methadone in human urine using solid-phase microextraction (SPME) and gas chromatography with nitrogen-phosphorus detection (GC-NPD). After the analytes had been partitioned between an extracting phase and the aqueous sample matrix, the needle of the coating fiber assembly was injected directly into the GC injector. The analytes were thermally desorbed in the heated injector (240 degrees C) and subsequently separated and detected by the GC-NPD system. The factors influencing the SPME method, such as the salt (NaCl) effect (15%), pH (pH 11), and equilibration time (30 min), were optimized. The calibration graphs for urine samples showed a good linearity. The detection limit was below 1 ng ml-1 for both drugs.

Determination of carphedon in human urine by solid-phase microextraction using capillary gas chromatography with nitrogen-phosphorus detection.

Carphedon is a phenyl derivative of nootropil and is effective in increasing physical endurance and cold resistance, and is used for amnesia treatment. Carphedon was extracted from human urine samples by solid-phase microextraction with a 65 microns carbowax-divinylbenzene-coated fiber. This analysis was performed by using capillary gas chromatography with nitrogen-phosphorus detection and optimized at pH 9.6, 30% NaCl, immersion time 10 min and desorption in the GC injector at 250 degrees C for 3 min. The regression equation for carphedon showed good linearity in the range from 0.1 to 10 micrograms ml-1 for human urine samples. The limit of detection was 0.01 microgram ml-1. The developed method is more sensitive and simpler in sample preparation than liquid-liquid extraction and can be applied to doping analysis for stimulants.

Determination of amphetamine, methamphetamine and dimethamphetamine in human urine by solid-phase microextraction (SPME)-gas chromatography/mass spectrometry.

A simple and rapid assay method for three stimulant drugs (amphetamine, methamphetamine, and dimethamphetamine) in human urine using solid-phase microextraction was developed. In solid-phase microextraction, the drugs were equilibrated between the adsorbent coated-fiber and aqueous sample matrix. After adsorption of the analytes, the fiber was directly transferred to the injector of a gas chromatograph, where the analytes were thermally desorbed and subsequently separated by the gas chromatograph and detected by mass spectrometer. The solid-phase microextraction method, which did not require solvents, was found to be a fast and simple analytical method. We optimized the solid-phase microextraction technique, for factors such as the NaCl salt effect (30%), pH effect (pH=12.4), equilibration time (30 min), desorption time (1 min) and coated-fiber type (100 microm poly(dimethylsiloxane)) and detected the stimulants in human urine, obtained from human subjects. The detection limits of each drug were below 1-10 ng/ml. The developed method can be applied to the abused drug test.

Gas chromatographic profiling and pattern recognition analysis of urinary organic acids from uterine myoma patients and cervical cancer patients.

An efficient organic acid profiling and pattern recognition method is described for the correlation between urinary organic acid profiles and uterine cervical cancer. After methoximation of keto acids in alkalinized urine samples, all free organic acids were recovered by a dual solid-phase extraction procedure, followed by conversion to tert.-butyldimethylsilyl derivatives for the profiling analysis by dual-capillary column gas chromatography (GC) with subsequent screening for acids by retention index (I) library matching. A total of 50 organic acids were positively identified in urine samples (0.25 ml) from 12 uterine myoma (benign tumor group) and 14 uterine cervical cancer (malignant tumor group) patients studied. When the GC profiles were simplified to their corresponding organic acid I spectra in bar graphical form, characteristic patterns were obtained for each average of benign and malignant tumor groups. Stepwise discriminant analysis performed on the GC data selected 16 acids as the variables discriminating between the two groups. Canonical discriminant analysis applied to these 16 variables correctly classified 26 urine samples into two separate clusters according to tumor types in the canonical plot.

Genotoxicity study of bojungchisup-tang, an oriental herbal decoction-in vitro chromosome aberration assay in Chinese hamster lung cells and in vivo supravital-staining micronucleus assay with mouse peripheral reticulocytes.

The toxicity evaluation of oriental herbal drugs is of great concern at present. Bojungchisuptang (BCST, in Korean), a decocted medicine of oriental herbal mixture, is now well used in clinic at oriental hospitals for the treatment of edema of several diseases in practice. However, the toxicity of the oriental herbal decocted medicines such as genetic toxicity is not well defined until now. In this respect, to clarify the genetic toxicity of BCST, in vitro chromosome aberration assay with Chinese hamster lung (CHL) fibroblasts and in vivo supravital micronucleus assay with mouse peripheral reticulocytes were performed in this study. In the chromosome aberration assay, we used 5,000 micrograms/ml BCST as maximum concentration because no remarkable cytotoxicity in CHL cells was observed both in the presence and absence of S-9 metabolic activation system. No statistical significant differences of chromosome aberrations were observed in CHL cells treated with 5,000, 2,500 and 1,250 micrograms/ml BCST for 6 hour both in the presence and absence of S-9 metabolic activation. However, very weak positive result (6.5-8.0% aberration) of BCST was obtained in the absence of S-9 metabolic activation system at 5,000 micrograms/ml BCST when treated for 24 hour, i.e. 1.5 normal cell cycle time. And also, in vivo clastogenicity of BCST was studied by acridine orange-supravital staining micronucleus assay using mouse peripheral reticulocytes. We used 2,000 mg/kg as the highest oral dose in this micronucleus assay because no acute oral toxicity of BCST was observed in mice. The optimum induction time of micronucleated reticulocytes (MNRETs) was determined as 36 hours after oral administration of 2,000 mg/kg BCST. No significant differences of MNRETs between control and BCST treatment groups were observed in vivo micronucleus assay. From these results, BCST revealed very weak positive result in chromosome aberration assay in vitro with CHL cells and no clastogenicity in micronucleus assay in vivo.

Identification of YH439 and its metabolites in rat urine by gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry.

YH439 is a potential drug candidate for the treatment of various hepatic disorders. YH439 and its three metabolites have been identified in rat urine by liquid chromatography-mass spectrometry (LC-MS) and by gas chromatography (GC)-MS. Identification of YH439 and its metabolites was established by comparing their GC retention times and mass spectra with those of the synthesized authentic standards. Both electron impact- and positive chemical ionization MS have been evaluated. The metabolism study was performed in the rat using oral administration of the drug. A major metabolite (YH438) was identified as the N-dealkylation product of YH439. Other identified metabolites were caused by the loss of the methyl thiazolyl amine group (metabolite II) from YH439, the isopropyl hydrogen malonate group (metabolite IV) and the decarboxylated product (metabolite III) of metabolite II.

Gas chromatographic-electron-impact chemical ionization mass spectrometric identification of cinmetacin and its metabolites in human urine.

Cinmetacin and its three metabolites were identified by gas chromatography-electron-impact positive-ion chemical ionization-negative chemical ionization mass spectrometry. After a single oral dose of 30 mg of cinmetacin to a healthy man, urine was collected and hydrolysed. The three metabolites were identified as O-desmethylated, N-descinnamoyl and C-C double bond reduced cinmetacins. The identification of cinmetacin metabolites in human urine was established by comparison of their GC retention times and electron impact and methane chemical ionization mass spectra with those of the synthesized authentic standards.