Chemical Composition and in vitro Anti-inflammatory Activity of Wheat Germ Oil Depending on the Extraction Procedure.

This study aimed to examine the chemical composition of wheat germ oil extracted by three different methods, and to evaluate its inhibitory effect on the cyclooxygenase and proteinase activities. The results showed that the contents of policosanols, tocopherols and phytosterols were affected by the extraction procedure. However, the fatty acid composition of the different oil extracts was nearly the same. Among the tested oils samples, cold pressed oil exhibited the strongest inhibitory activity against proteinase (93.4%, IC50 =195.7 µg/mL) and cyclooxygenase 1 (80.5%, IC50 =58.6 µg/mL). Furthermore, the cold pressed oil had the highest content of octacosanol, ß-sitosterol and α-linolenic acid, suggesting that those bioactive compounds could be essential for the potent ani-cyclooxygenase activity. The present data revealed that wheat germ oil contained cyclooxygenase and trypsin inhibitors, which are the promising therapeutic target for the treatment of various inflammatory diseases. Thus, wheat germ oil might be used to develop functional foods and pharmaceutic products for the human health.

Spectral characterization, antioxidant, antimicrobial, cytotoxic, and cyclooxygenase inhibitory activities of Aloysia citriodora essential oils collected from two Palestinian regions.

BACKGROUND: Aloysia citriodora Palau (AC) is commonly known as Lemon Verbena and has been utilized as a medicinal tea in folkloric medicine for the treatment of abdominal spasm, anxiety, and fever. The present investigation aimed to identify the chemical ingredients of AC essential oil (EO) collected from two different locations in Palestine and to assess their antioxidant, antimicrobial, cytotoxic, and cyclooxygenase (COX) inhibitory effects. METHODS: Gas chromatography/mass spectroscopy (GC/MS) technique was used to identify the chemical components of the hydro-distilled EO from both regions, while DPPH, MTS, and COX assays were utilized to estimate the antioxidant, cytotoxic, and COX inhibitory activities of the EOs, respectively. Moreover, a broth microdilution assay was used to assess antimicrobial potentials against seven microbial strains. RESULTS: The GC/MS technique revealed the presence of 17 compounds from the AC collected from the Umm al-Fahm region and 13 compounds from the sample from the Baqa al-Gharbiyye region, while α-citral was the major component of both EOs, representing 47.62 and 43.46%, respectively. The Baqa al-Gharbiyye AC EO exerted more potent antioxidant activity than the Umm al-Fahm EO, with IC50 values of 11.74 ± 0.18 and 35.48 ± 0.14 µg/mL, respectively, while the positive control Trolox had antioxidant IC50 values of 2.45 ± 0.01 µg/mL. Interestingly, both EOs inhibited more potential activity against Methicillin-Resistant Staphylococcus aureus (MRSA) and Proteus vulgaris than Ciprofloxacin and Ampicillin antibiotics and also showed more potent antifungal activity against Candida albicans than Fluconazole. Moreover, the Baqa al-Gharbiyye AC EO had a more potent cytotoxic effect than the Umm al-Fahm EO, with IC50 values of 84.5 ± 0.24 and 33.31 ± 0.01 µg/mL, respectively, compared with Doxorubicin, which had an IC50 dose of 22.01 ± 1.4 µg/mL. The EOs from Baqa al-Gharbiyye showed potent activity against both COX-1 and COX-2 enzymes, with IC50 of 52.93 ± 0.13 and 89.31 ± 0.21 µg/mL, respectively, while the EOs from the Umm al-Fahm region showed weaker activity against these enzymes, with IC50 of 349.99 ± 0.33 and 1326.37 ± 1.13 µg/mL, respectively. CONCLUSION: Both characterized EOs have a huge variety of chemical components. The Baqa al-Gharbiyye AC EO has more potent antioxidant and cytotoxic activities than the Umm al-Fahm EO, but both have potential antimicrobial activity against MRSA, P. vulgaris, and C. albicans. These results suggest the use of AC EOs as promising sources of active ingredients in the food, cosmetic, and pharmaceutical industries.

[Determination of seven non-selective cyclooxygenase inhibitors in milk powder by ultra-performance liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction].

An ultra-performance liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction (dSPE-UPLC-MS/MS) method was developed to determine seven non-selective cyclooxygenase inhibitors in milk powder. The samples were extracted with 0.01 mol/L pH 2.5 ascorbic acid-acetonitrile-ethyl acetate solution (2:5:5, v/v/v), and then purified with a mixture of anhydrous sodium sulfate, octadecyl carbon silica gel (C18-N) sorbent and ethylenediamine-N-propyl carbon silica gel (NH2-PSA) sorbent. The analysis was performed using a UPLC-MS/MS system with Waters CORTECS UPLC C18 (100 mm×2.1 mm, 1.6 µm) column. The mobile phase consisted of 0.1% (v/v) formic acid aqueous solution and acetonitrile containing 0.1% (v/v) formic acid by gradient elution, and the multiple reaction monitoring (MRM) mode was used. Five linear calibration curves were obtained with correlation coefficients (r2) ≥ 0.9965. The recoveries were determined at three spiked levels and ranged from 76.4% to 89.8%. The limits of quantification (LOQs) were from 2 to 5 µg/kg. This method is suitable for the determination of seven non-selective cyclooxygenase inhibitors in milk powder.

A comparative study of the novel spectrophotometric methods versus conventional ones for the simultaneous determination of Esomeprazole magnesium trihydrate and Naproxen in their binary mixture.

Two novel simple, specific, accurate and precise spectrophotometric methods manipulating ratio spectra are developed and validated for simultaneous determination of Esomeprazole magnesium trihydrate (ESO) and Naproxen (NAP) namely; absorbance subtraction and ratio difference. The results were compared to that of the conventional spectrophotometric methods namely; dual wavelength and isoabsorptive point coupled with first derivative of ratio spectra and derivative ratio. The suggested methods were validated in compliance with the ICH guidelines and were successfully applied for determination of ESO and NAP in their laboratory prepared mixtures and pharmaceutical preparation. No preliminary separation steps are required for the proposed spectrophotometeric procedures. The statistical comparison showed that there is no significant difference between the proposed methods and the reported method with respect to both accuracy and precision.

Bioactive properties of commercialised pomegranate (Punica granatum) juice: antioxidant, antiproliferative and enzyme inhibiting activities.

Pomegranate juice and related products have long been used either in traditional medicine or as nutritional supplements claiming beneficial effects. Although there are several studies on this food plant, only a few studies have been performed with pomegranate juice or marketed products. The aim of this work is to evaluate the antioxidant effects of pomegranate juice on cellular models using hydrogen peroxide as an oxidizing agent or DPPH and superoxide radicals in cell free systems. The antiproliferative effects of the juice were measured on HeLa and PC-3 cells by the MTT assay and pharmacologically relevant enzymes (cyclooxygenases, xanthine oxidase, acetylcholinesterase and monoamine oxidase A) were selected for enzymatic inhibition assays. Pomegranate juice showed significant protective effects against hydrogen peroxide induced toxicity in the Artemia salina and HepG2 models; these effects may be attributed to radical scavenging properties of pomegranate as the juice was able to reduce DPPH and superoxide radicals. Moderate antiproliferative activities in HeLa and PC-3 cancer cells were observed. However, pomegranate juice was also able to inhibit COX-2 and MAO-A enzymes. This study reveals some mechanisms by which pomegranate juice may have interesting and beneficial effects in human health.

Solid phase microextraction of diclofenac using molecularly imprinted polymer sorbent in hollow fiber combined with fiber optic-linear array spectrophotometry.

A simple solid phase microextraction method based on molecularly imprinted polymer sorbent in the hollow fiber (MIP-HF-SPME) combined with fiber optic-linear array spectrophotometer has been applied for the extraction and determination of diclofenac in environmental and biological samples. The effects of different parameters such as pH, times of extraction, type and volume of the organic solvent, stirring rate and donor phase volume on the extraction efficiency of the diclofenac were investigated and optimized. Under the optimal conditions, the calibration graph was linear (r(2)=0.998) in the range of 3.0-85.0 µg L(-1) with a detection limit of 0.7 µg L(-1) for preconcentration of 25.0 mL of the sample and the relative standard deviation (n=6) less than 5%. This method was applied successfully for the extraction and determination of diclofenac in different matrices (water, urine and plasma) and accuracy was examined through the recovery experiments.

Anti-inflammatory activity of copao (Eulychnia acida Phil., Cactaceae) fruits.

Copao (Eulychnia acida Phil., Cactaceae) is an endemic species occurring in northern Chile. The edible fruits of this plant are valued for its acidic and refreshing taste. Phenolic-enriched extracts from copao fruit pulp and epicarp, collected in the Elqui and Limari river valleys, were assessed by its in vitro ability to inhibit the pro-inflammatory enzymes lipoxygenase (LOX) and cyclooxygenases (COX-1 and COX-2). At 100 µg/mL, pulp extracts showed better effect towards LOX than epicarp extract, while COX-2 inhibition was observed for both epicarp and pulp samples. In general, the extracts were inactive towards COX-1. A positive correlation was observed between the anti-inflammatory activity and the main phenolic compounds found in this fruit. Copao fruits from the Limari valley, a main place of collection and commercialization, showed major activity, adding evidence on the possible health-beneficial effects of this native Chilean fruit.

Functionalized magnetic nanoparticles coupled with mass spectrometry for screening and identification of cyclooxygenase-1 inhibitors from natural products.

Development of simple and effective methods for high-throughput, high-fidelity screening and identification of cyclooxygenase-1 (COX-1) inhibitors from natural products are important for drug discovery to treat inflammation and carcinogenesis. Here, we developed a new screening assay based on cyclooxygenase-1 (COX-1) functionalized magnetic nanoparticles (i.e. Fe3O4@SiO2-COX-1) for solid phase ligand fishing, and then mass spectrometry (MS) was applied for structural identification. Incubation conditions were optimized. High specificity for isolating COX-1 inhibitors was achieved by testing positive control, indomethacin, with active and inactive COX-1. Moreover, high stability of immobilized COX-1 (remained 95.3% after ten consecutive cycles) allows the analysis reproducible. When applied to turmeric extract, four curcuminoids (i.e. curcumin, demethoxycurcumin, bisdemethoxycurcumin, and 1-(4-hydroxy-3,5-dimethoxyphenyl)-7-(4-hydroxy-3-methoxyphenyl)-(1E,6E)-1,6-heptadiene-3,5-dione), difficult to be distinguished from original MS spectrum of turmeric extract, were isolated as main COX-1 inhibitors. Their structures were characterized based on their accurate molecular weight and diagnostic fragment ions. The results indicated that the proposed method was a simple, robust and reproducible approach for the discovery of COX-1 inhibitors from complex matrixes.

Ardisia crispa roots inhibit cyclooxygenase and suppress angiogenesis.

BACKGROUND: In our previous studies conducted on Ardisia crispa roots, it was shown that Ardisia crispa root inhibited inflammation-induced angiogenesis in vivo. The present study was conducted to identify whether the anti-angiogenic properties of Ardisia crispa roots was partly due to either cyclooxygenase (COX) or/and lipoxygenase (LOX) activity inhibition in separate in vitro studies. METHODS: Benzoquinonoid fraction (BQ) was isolated from hexane extract by column chromatography, and later analyzed by using gas chromatography-mass spectrometry (GC-MS). Anti-angiogenic effect was studied on mouse sponge implantation assay. Ardisia crispa ethanolic rich fraction (ACRH), quinone-rich fraction (QRF) and BQ were screened for COX assay to evaluate their selectivity towards two isoforms (COX-1 and COX-2), The experiment on soy lipoxygenase (LOX) inhibitory assay was also performed to determine the inhibitory effect of ACRH, QRF and BQ on soy LOX. RESULTS: BQ was confirmed to consist of 2-methoxy-6-undecyl-1,4-benzoquinone, when compared with previous data. Antiangiogenesis study exhibited a reduction of mean vascular density (MVD) in both ACRH and QRF, compared to control. In vitro study showed that both ACRH and QRF inhibited both COX-1 and COX-2, despite COX-2 inhibition being slightly higher than COX-1 in BQ. On the other hand, both ACRH and QRF were shown to have poor LOX inhibitory activity, but not BQ. CONCLUSIONS: In conclusion, ACRH and QRF might possibly exhibit its anti-angiogenic effect by inhibiting cyclooxygenase. However, both of them were shown to possess poor LOX inhibitory activity. On the other hand, BQ displayed selectivity to COX-2 inhibitory property as well as LOX inhibitory effect.

Antioxidant and anti-inflammatory assays confirm bioactive compounds in Ajwa date fruit.

Ajwa, a variety of date palm Phoenix dactylifera L., produces the most expensive date fruits. Percentages of seed, moisture, fructose, glucose, soluble protein, and fiber in Ajwa dates were 13.24, 6.21, 39.06, 26.35, 1.33, and 11.01, respectively. The ethyl acetate, methanolic, and water extracts of Ajwa dates, active at 250 µg/mL in the MTT assay, inhibited lipid peroxidation (LPO) by 88, 70, and 91% at 250 µg/mL and cyclooxygenase enzymes COX-1 by 30, 31, and 32% and COX-2 by 59, 48, and 45% at 100 µg/mL, respectively. Bioactivity-guided purifications afforded compounds 1-7, in addition to phthalates and fatty acids. Compounds 1-3 showed activity at 100 µg/mL in the MTT assay; inhibited COX-1 enzyme by 59, 48, amd 50% and COX-2 enzyme by 60, 40, amd 39% at 50 µg/mL; and inhibited LPO by 95, 58, amd 66% at 100 µg/mL, respectively. The soluble protein fraction was also very active in both antioxidant and anti-inflammatory assays.

Phenolics content and antioxidant and anti-inflammatory activities of legume fractions.

Two faba bean (Vicia faba L.) subspecies major and minor and lentil seeds grown in Algeria were separated into cotyledons and hulls. These fractions, together with their corresponding whole seeds, were extracted with two solvents, aqueous (70%) acetone and (80%) ethanol, and evaluated for antioxidant activity in relation to their phenolic contents. Acetone selectively extracted tannins from faba beans. The hulls always exhibited high antioxidant activity, measured using the reducing power (RP), antiradical activity (DPPH) or oxygen radical absorbance capacity (ORAC) assays. Aqueous ethanol (80%) extract of lentil hulls exhibited high antioxidant and anti-inflammatory activities preferentially inhibiting 15-LOX (IC(50), 55 µg/ml), with moderate COX-1 (IC(50), 66 µg/ml) and COX-2 (IC(50), 119 µg/ml) inhibitory effects on the COX pathway, whereas faba bean hull extracts exerted relatively mild LOX inhibitory activity.

Investigation for the amorphous state of ER-34122, a dual 5-lipoxygenase/cyclooxygenase inhibitor with poor aqueous solubility, in HPMC solid dispersion prepared by the solvent evaporation method.

ER-34122, a poorly water-soluble dual 5-lipoxygenase/cyclooxygenase inhibitor, exists as a crystalline form. According to an Oak Ridge thermal ellipsoid plot drawing, carbonyl oxygen O (5) makes an intermolecular hydrogen bond with the hydrogen bonded to N (3) in the crystal structure. The FTIR and the solid-state ¹³C NMR spectra suggest that the network is spread out in the amorphous state and the hydrogen bonding gets weaker than that in the crystalline phase, because the carbonyl signals significantly shift in both spectra. When amorphous ER-34122 was heated, crystallization occurred at around 140°C. Similar crystallization happened in the solid dispersion; however, the degree of crystallization was much lower than that observed in the pure amorphous material. Also, the DSC thermogram of the solid dispersion did not show any exothermic peaks implying crystallization. The heat of fusion (ΔHf) determined in the pure amorphous material was nearly equal to that for the crystalline form, whereas the ΔHf value obtained in the solid dispersion was less than a third of them. These data prove that crystallization of the amorphous form is dramatically restrained in the solid dispersion system. The carbonyl wavenumber shifts in the FTIR spectra indicate that the average hydrogen bond in the solid dispersion is lower than that in the pure amorphous material. Therefore, HPMC will suppress formation of the intermolecular network observed in ER-34122 crystal and preserve the amorphous state, which is thermodynamically less stable, in the solid dispersed system.

TLC determination of meloxicam in tablets and after acidic and alkaline hydrolysis.

A simple and rapid method for separation and determination of meloxicam and its degradation products by thin-layer chromatography with densitometric detection in pharmaceutical preparations was described. The method employed TLC F254 plates as the stationary phase. The solvent system consisted of ethyl acetate : toluene : butylamine (2:2:1, v/v/v). Densitometric analysis was carried out in absorbance mode at wavelength of 297 nm. The method was validated for linearity, precision and accuracy. The limits of detection and determination were 0.96 µg per spot and 2.90 µg per spot, respectively. The drug was degraded in acidic and basic environment, at different temperatures. The degradation products were well resolved from the active substance. The HPLC-MS/MS method for the identification of degradation products of meloxicam (i.e. 5-methylthiazol- 2-ylamine and 5-(dioxide-l(6)-sulfanylidene)-6-methylidenecyclohexa-1,3-diene) was investigated. Because the presented method allows the efficient separation of the drug from some of its degradation products, so it can be used as a stability-indicating analysis.

Inhibitory effects of bioactive leads isolated from Pseudomonas aeruginosa PS3 and Pseudomonas fluorescens PS7 on MAP kinases and down regulation of pro inflammatory cytokines (TNF-α, IL-1ß) and mediators (NO, iNOS and COX).

Pure lead molecules, showing anti-inflammatory effect were isolated from the marine Pseudomonas aeruginosa PS3 (GenBank Accession No. EF488968) and Pseudomonas fluorescens PS7 (GenBank Accession No. EF488969) using solvent extraction procedures, subsequent column fractionation, followed by bio activity based screening. The structures of the lead molecules (3S, 8aS)-3-isobutylhexahydropyrrolo[1,2-a]pyrazine-1,4-dione (Compound 1) and (8aS)-3-(4-hydroxybenyl) hexahydropyrrolo[1,2-a]pyrazine-1,4-dione (Compound 2) obtained from P. aeruginosa PS3 and P. fluorescens PS7 respectively were established employing spectral analysis. Compounds 1 and 2 at their IC(50) values of 84 and 53µM concentrations respectively down regulated expression of tumor necrosis factor-α (TNF-α) and interleukin 1-ß (IL-1ß) in peripheral blood mononuclear cells (PBMCs) and inducible nitric oxide synthase (iNOS) gene in RAW 264.7 cells. Immunoblot analysis revealed the inhibitory effect of pure compounds on phosphorylation of all the three mitogen activated protein kinases (MAPK) such as ERK, JNK and p38 MAPK. The results of the present investigation revealed that the pure compounds are anti-inflammatory in nature.

Suppressive effect of short-chain fatty acids on production of proinflammatory mediators by neutrophils

Short chain fatty acids (SCFAs) are fermentation products of anaerobic bacteria. More than just being an important energy source for intestinal epithelial cells, these compounds are modulators of leukocyte function and potential targets for the development of new drugs. The aim of this study was to evaluate the effectsof SCFAs (acetate, propionate and butyrate) on production of nitric oxide (NO) and proinflammatory cytokines [tumor necrosis factor á (TNF-á) and cytokineinduced neutrophil chemoattractant-2 (CINC-2áâ)] by rat neutrophils. The involvement of nuclear factor êB (NF-êB) and histone deacetylase (HDAC) wasexamined. The effect of butyrate was also investigated in vivo after oral administration of tributyrin (a pro-drug of butyrate). Propionate and butyrate diminished TNF-á, CINC-2áâ and NO production by LPS-stimulated neutrophils. We also observed that these fatty acids inhibit HDAC activity and NF-êB activation, which might be involved in the attenuation of the LPS response. Products of cyclooxygenase and 5-lipoxygenase are not involved in the effects of SCFAs as indicated by the results obtained with the inhibitors of these enzymes. The recruitment of neutrophils to the peritonium after intraperitoneal administration of a glycogen solution (1%) and the ex vivo production of cytokines and NO by neutrophils were attenuated in rats that previously received tributyrin. These results argue that this triglyceride may be effective in the treatment of inflammatory conditions.

Spherical harmonics coefficients for ligand-based virtual screening of cyclooxygenase inhibitors.

BACKGROUND: Molecular descriptors are essential for many applications in computational chemistry, such as ligand-based similarity searching. Spherical harmonics have previously been suggested as comprehensive descriptors of molecular structure and properties. We investigate a spherical harmonics descriptor for shape-based virtual screening. METHODOLOGY/PRINCIPAL FINDINGS: We introduce and validate a partially rotation-invariant three-dimensional molecular shape descriptor based on the norm of spherical harmonics expansion coefficients. Using this molecular representation, we parameterize molecular surfaces, i.e., isosurfaces of spatial molecular property distributions. We validate the shape descriptor in a comprehensive retrospective virtual screening experiment. In a prospective study, we virtually screen a large compound library for cyclooxygenase inhibitors, using a self-organizing map as a pre-filter and the shape descriptor for candidate prioritization. CONCLUSIONS/SIGNIFICANCE: 12 compounds were tested in vitro for direct enzyme inhibition and in a whole blood assay. Active compounds containing a triazole scaffold were identified as direct cyclooxygenase-1 inhibitors. This outcome corroborates the usefulness of spherical harmonics for representation of molecular shape in virtual screening of large compound collections. The combination of pharmacophore and shape-based filtering of screening candidates proved to be a straightforward approach to finding novel bioactive chemotypes with minimal experimental effort.

Identification and quantification of a major anti-oxidant and anti-inflammatory phenolic compound found in basil, lemon thyme, mint, oregano, rosemary, sage, and thyme.

Major phenolic compounds from basil, lemon thyme, mint, oregano, rosemary, sage, and thyme were investigated using a high-performance liquid chromatography (HPLC) profiling technique in combination with DPPH-radical scavenging, xanthine oxidase and cyclooxygenase assays. For the present study, 15 plant-derived phenolic compounds (gallic, protocatechuic, vanillic, syringic, chlorogenic, rosmarinic, caffeic, ferulic, and sinapic acids, protocatechualdehyde, vanillin, N-coumaroyltyramine, N-caffeoyltyramine, N-feruloyltyramine, and N-sinapoyltyramine) were selected and their DPPH-radical scavenging activities were first determined. Then, a standard HPLC profiling of these phenolics was constructed using an HPLC method to isolate anti-oxidant and anti-inflammatory phenolic compounds from MeOH extracts of the plants. Rosmarinic acid was identified as a major anti-oxidant compound (0.22-0.97%) in all seven herbs, confirmed by nuclear magnetic resonance. Rosmarinic acid from the plants quenched superoxide radicals from xanthine oxidase and inhibited cyclooxygenase I and II enzymes. In this study, the rosmarinic acid content of perilla was also determined and compared with those of the seven herbs.

Anti-inflammatory, antioxidant, anti-tyrosinase and phenolic contents of four Podocarpus species used in traditional medicine in South Africa.

ETHNOPHARMACOLOGICAL RELEVANCE: Species of Podocarpus are used traditionally in their native areas for the treatment of fevers, asthma, coughs, cholera, chest complaints, arthritis, rheumatism, venereal diseases and distemper in dogs. AIMS OF THE STUDY: To investigate the antioxidant, anti-inflammatory and anti-tyrosinase activities of four Podocarpus species, Podocarpus elongatus, Podocarpus falcatus, Podocarpus henkelii and Podocarpus latifolius, used in traditional medicine in South Africa. Phytochemical analysis to determine the phenolic contents was also carried out. MATERIALS AND METHODS: DPPH, FRAP and ß-carotene-linoleic acid assays were used to determine the antioxidant/radical scavenging activities of these species. Anti-inflammatory activity of these species was assayed against two cyclooxygenase enzymes (COX-1 and COX-2). Tyrosinase inhibition activity was analysed using the modified dopachrome method with l-DOPA as the substrate. Phenolics were quantitatively determined using spectrophotometric methods. RESULTS: Stems of Podocarpus latifolius exhibited the lowest EC(50) (0.84 µg/ml) inhibition against DPPH. The percentage antioxidant activity based on the bleaching rate of ß-carotene ranged from 96% to 99%. High ferric reducing power was observed in all the extracts. For COX-1, the lowest EC(50) value was exhibited by stem extracts of Podocarpus elongatus (5.02 µg/ml) and leaf extract of Podocarpus latifolius showed the lowest EC(50) against COX-2 (5.13 µg/ml). All extracts inhibited tyrosinase activity in a dose-dependent manner with stem extract of Podocarpus elongatus being the most potent with an EC(50) value of 0.14 mg/ml. The total phenolic content ranged from 2.38 to 6.94 mg of GAE/g dry sample. CONCLUSION: The significant pharmacological activities observed support the use of these species in traditional medicine and may also be candidates in the search for modern pharmaceuticals in medicine, food and cosmetic industries.

[Turbidimetric determination of tenoxicam using molybdophosphoric acid]. / Determinarea turbididimetrica a tenoxicamului folosind ca reactiv solutia de acid fosfomolibdenic.

UNLABELLED: A turbidimetric method was developed for tenoxicam quantification using the complexing reaction with molybdophosphoric acid in hydrochloric acid medium; the complex has a maximum of absorbance at 369 nm. MATERIALS AND METHOD: The practical working conditions were established. In the 2.5 division by 15.0 microg/mL concentration range of tenoxicam in 1N hydrochloric acid, were added 1 mL of 1% molybdophosphoric acid solution and 1 mL of 0.1% sodium lauryl sulphate. The stability of product was evaluated over 60 minutes. The developed method was validated. RESULTS: The method showed a good linearity in the range of 2.5 division by 15.0 microg/mL (the correlation coefficient r = 0.9996). The detection limit (LD) was 0.44 microg/mL and the quantification limit (LQ) was 1.47 microg/mL. There were established the precision (RSD = 1.82%) and the accuracy (mean recovery is 100.79% in 97.55 division by BY 04.41% the range). CONCLUSIONS: The experimental results demonstrated a good sensibility. The specific absorptivity for this method is A(1cm,369nm)(1%) higher than tenoxicam in hydrochloric acid medium A(1cm,354nm)(1%).

In vitro cyclooxygenase inhibition assay for evaluating ecotoxicity of the surface water and domestic wastewater in the Tone Canal, Japan.

Cyclooxygenase (COX) plays an important role in eicosanoid metabolism. Nonsteroidal anti-inflammatory drugs (NSAIDs) function as COX inhibitors and are frequently detected in the aquatic environment. Here, we measured the in vitro COX-inhibiting activity of the surface water and domestic wastewater in the Tone Canal, Japan. The concentrations of several NSAIDs in the some samples were also determined using gas chromatography-tandem mass spectrometry for confirming the validity of the assay. The target compounds were extracted from the samples using a solid-phase extraction cartridge. A dose-response relationship between the inhibiting activity and sample volume were observed in the wastewater sample. The higher COX-inhibiting activities were observed in the wastewater sample, as compared with the samples of the surface water in the canal. These inhibiting activities reflected the trends of NSAIDs distribution in the canal. However, the inhibiting activities of the water samples could not be entirely explained by the NSAIDs that were selected for instrumental analysis in this study. Other compounds that were not measured by instrumental analysis in this study might contribute to the inhibiting activities. Therefore, the COX-inhibiting assay would be effective for evaluating inclusive ecotoxicity in the aquatic environment.