Processing of high performance composites based on peek by aqueous suspension prepregging

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Determination of pesticide residues in coconut water by liquid-liquid extraction and gas chromatography with electron-capture plus thermionic specific detection and solid-phase extraction and high-performance liquid chromatography with ultraviolet detection

Two simple methods were developed to determine, 11 pesticides in coconut water, a natural isotonic drink rich in salts, sugars and vitamins consumed by the people and athletes. The first procedure involves solid-phase extraction using Sep-Pak Vac C-18 disposable cartridges with methanol for elution. Isocratic analysis was carried out by means of high-performance liquid chromatography with ultraviolet detection at 254 nm to analyse captan, chlorothalonil, carbendazim, lufenuron and diafenthiuron. The other procedure is based on liquid-liquid extraction with hexane-dichloromethane (1:1, v/v), followed by gas chromatographic analysis with effluent splitting to electron-capture detection for determination of endosulfan, captan, tetradifon and trichlorfon and thermionic specific detection for determination of malathion, parathion-methyl and monocrotophos. The methods were validated with fortified samples at different concentration levels (0.01-12.0 mg/kg). Average recoveries ranged from 75 to 104% with relative standard deviations between 1.4 and 11.5%. Each recovery analysis was repeated at least five times. Limits of detection ranged from 0.002 to 2.0 mg/kg. The analytical procedures were applied to 15 samples and no detectable amounts of the pesticides were found in any samples under the conditions described. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Quantitative determination of anti-fungal and insecticide amides in adult plants, plantlets and callus from Piper tuberculatum by reverse-phase high-performance liquid chromatography

A rapid, sensitive and reliable reverse-phase HPLC method was used for the quantitative determination of the anti-fungal and insecticide amides, dihydropiplartine (1), piplartine (2), Delta(alpha,beta)-dihydropiperine (3) and pellitorine (4) in plants in natura, in plantlets in vitro and ex vitro, and in callus of Piper tuberculatum. Well-resolved peaks were obtained with good detection response and linearity in the range of 15.0-3000 mug/mL. The plants in natura contained compounds 1-4, the plantlets ex vitro and in vitro accumulated compounds 1-2 and 1-4, respectively, while only amide 4 was found in callus. Copyright (C) 2003 John Wiley Sons, Ltd.

Quantitative determination of maitenin and 22 beta-hydroxymaitenin in callus of Maytenus aquifolium (Celastraceae) by reverse phase high performance liquid chromatography

Explants of Maytenus aquifolium were induced to form callus and, subsequently, suspension cultures. The isolation of natural products from callus led to the identification of the cytotoxic triterpene quinonemethides, maitenin (1) and 22 beta-hydroxymaitenin (2), A rapid, sensitive and reliable reversed-phase high-performance liquid chromatography method was developed using a Cls column and isocratic elution for the determination of 1 and 2, the elaborated method gave well-resolved peaks for these compounds with good detection response and linearity in the range of 0.08-72.0 mu g. The quantification of 1 and 2 was performed by an external standard method. (C) 1998 John Wiley & Sons, Ltd.

Determination of the betaine content of feed ingredients using high-performance liquid chromatography

A series of studies was conducted to establish a methodology for the accurate and efficient determination of betaine in different feed ingredients. The final methodology involves an extraction step in which the feed sample is heated for 3h in a methanolic KOH solution using a Goldfisch apparatus. Impurities are removed by the addition of activated charcoal and concentrated (36%) HCl. After centrifugation the extractant is passed through a strong cation exchange resin (Dowex 50W-X12, H+). The betaine retained in the column is eluted with 1.5 N HCl. A 2 nil aliquot of the elute is air dried and reconstituted with 1 ml of deionised water. HPLC separation with a cation exchange column (Partisil SCX-10) is used for the separation of betaine from other compounds. The mobile phase is kept constant at 50mm KH2PO4 in water, and eluted compounds are detected by UV absorbance (200nm). The flow rate is maintained at 1.5ml min(-1). This assay is very accurate over the range of betaine concentrations from 15 to 650 mug ml(-1), with a lower detection limit in feeds of approximately 500 mug g(-1) when 4g of sample is extracted. Recovery assays done with standard betaine hydrochloride and hard red wheat resulted in a consistent recovery of 80%. Betaine content was quantified in several feed ingredients, including alfalfa (1.77 mg kg(-1)), wheat (3.96 mg kg(-1)), wheat middlings (4.98 mg kg(-1)) and poultry meal (0.77 mg kg(-1)). Betaine in corn and soybean meal was not detectable by this method, even when 16g of sample was used (<125 mg kg(-1)). Betaine present in several feed ingredients should influence choline supplementation to animal feeds and may have implications for human health. (C) 2002 Society of Chemical Industry.

Comparison of different clean-up procedures for the determination of N-methylcarbamate insecticides in vegetable matrices by high-performance liquid chromatography with UV detection

Several clean-up procedures which included the use of glass chromatography columns (silica gel, alumina, Florisil, silanized Celite-charcoal), Sep-Pak cartridges and standard solutions were compared for the determination of the following N-methylcarbamate (NMC) insecticides: aldicarb, carbaryl, carbofuran, methomyl and propoxur. According to recovery results of the compounds after elution in a glass column, the most efficient systems employed 4.6% deactivated alumina and a silanized Celite-charcoal (4:1) as adsorbents, using dichloromethane-methanol (99:1) and toluene-acetonitrile (75:25) mixtures, respectively, as binary eluents. The recoveries of the compounds studied varied from 84 to 120%. Comparable recoveries (75-100%) for Sep-Pak cartridges in normal phase (NH2, CN) and reversed phase (C-8) were observed. Different temperatures were tested during the concentration step in a rotary evaporator, and we verified a strong influence of this parameter on the stability of some compounds, such as carbofuran and carbaryl. Recovery studies employing the best clean up procedures were performed at the Brazilian agricultural level in potato and carrot samples; Validation methodology of the US Food and Drug Administration was adapted for the N-methylcarbamate analysis. Their recoveries ranged between 79 and 93% with coefficients of variation of 2.3-8%. (C) 1998 Elsevier B.V. B.V.

Rapid and sensitive method for the determination of acetaldehyde in fuel ethanol by high-performance liquid chromatography with UV-Vis detection

A high-performance liquid chromatography (HPLC) method for the determination of acetaldehyde in fuel ethanol was developed. Acetaldehyde was derivatized with 0.900 mL 2,4-dinitrophenylhydrazine (DNPHi) reagent and 50 mu L phosphoric acid 1 mol L-1 at a controlled room temperature of 15 degrees C for 20 min. The separation of acetaldehyde- DNPH (ADNPH) was carried out on a Shimadzu Shim-pack C-18 column, using methanol/LiCl(aq) 1.0 mM (80/20, v/v) as a mobile phase under isocratic elution and UV-Vis detection at 365 nm. The standard curve of ADNPH was linear in the range 3-300 amg L-1 per injection (20 mu L) and the limit of detection (LOD) for acetaldehyde was 2.03 mu g L-1, with a correlation coefficient greater than 0.999 and a precision (relative standard deviation, RSD) of 5.6% (n=5). Recovery studies were performed by fortifying fuel samples with acetaldehyde at various concentrations and the results were in the range 98.7-102%, with a coefficient of variation (CV) from 0.2% to 7.2%. Several fuel samples collected from various gas stations were analyzed and the method was successfully applied to the analysis of acetaldehyde in fuel ethanol samples.

A high-performance liquid chromatographic assay for sparfloxacin

A specific and sensitive high-performance liquid chromatographic procedure was developed for the assay of sparfloxacin in raw material and tablets. It was also found that the excipients in the commercial tablet preparation did not interfere with the assay. The method validation yielded good results and included the range, linearity, precision, accuracy, specificity and recovery. This method can also be applied to stability studies. (C) 1999 Elsevier B.V. B.V. All rights reserved.

Quantitative determination of cytotoxic friedo-nor-oleanane derivatives from five morphological types of Maytenus ilicifolia (Celastraceae) by reverse-phase high-performance liquid chromatography

Five different morphological types of Maytenus ilicifolia of the same age and harvested under the same conditions showed distinct accumulations of some friedo-nor-oleananes. A rapid, sensitive and reliable reverse-phase HPLC method (employing an external standard) was used for the determination of the cytotoxic triterpenoids, 20alpha-hydroxymaytenin, 22beta-hydroxymaytenin, maytenin, celastrol and pristimerin in each of the five types. Well resolved peaks with good detection response and linearity in the range 1.0-100 mug/mL were obtained. Copyright (C) 2002 John Wiley Sons, Ltd.

Determination of aldicarb, aldicarb sulfoxide and aldicarb sulfone in some fruits and vegetables using high-performance liquid chromatography-atmospheric pressure chemical ionization mass spectrometry

An analytical method for the determination of aldicarb, and its two major metabolites, aldicarb sulfoxide and aldicarb sulfone in fruits and vegetables is described. Briefly the method consisted of the use of a methanolic extraction, liquid-liquid extraction followed by solid-phase extraction clean-up. Afterwards, the final extract is analyzed by liquid chromatography-atmospheric pressure chemical ionization mass spectrometry (LC-APCI-MS). The specific fragment ion corresponding to [M-74](+) and the protonated molecular [M+K](+) ion were used for the unequivocal determination of aldicarb and its two major metabolites. The analytical performance of the proposed method and the results achieved were compared with those obtained using the common analytical method involving LC with post-column fluorescence detection (FL). The limits of detection varied between 0.2 and 1.3 ng but under LC-FL were slightly lower than when using LC-APCI-MS. However both methods permitted one to achieve the desired sensitivity for analyzing aldicarb and its metabolites in vegetables. The method developed in this work was applied to the trace determination of aldicarb and its metabolites in crop and orange extracts. (C) 2000 Elsevier B.V. B.V. All rights reserved.

Simultaneous determination of furanocoumarins in infusions and decoctions from Carapia (Dorstenia species) by high-performance liquid chromatography

The use of furanocoumarins, which are photosensitizing compounds, combined with exposure to UV-A radiation is a common treatment for vitiligo, psoriasis, and a number of other skin diseases. Although furanocoumarins plus UV-A treatment is highly effective, several studies have shown that exposure to high doses increases the risk to development of cutaneus carcinoma. Several Dorstenia species are used in folk medicine, mainly against skin diseases, because of the presence of biologically active compounds. We present here analysis of the chemical composition of furanocoumarins from infusion and decoction of Carapia (Dorstenia species), which is used in Brazil against several diseases. We have employed high-performance liquid chromatography (HPLC) procedures for the quantitative determination of psoralen, bergapten, and isopimpinellin. The contents of furanocoumarins revealed an insignificant difference between infusion and decoction. Dorstenia tubicina and D. asaroides contained psoralen and bergapten only in the rhizomes, whereas D. vitifolia shows solely isopimpinellin in both rhizomes and aerial parts.

Determination of acetaldehyde in fuel ethanol by high-performance liquid chromatography with electrochemical detection

The cyclic voltammetric behavior of acetaldehyde and the derivatized product with 2,4-dinitrophenylhydrazine (DNPHi) has been studied at a glassy carbon electrode. This study was used to optimize the best experimental conditions for its determination by high-performance liquid chromatographic (HPLC) separation coupled with electrochemical detection. The acetaldehyde-2,4-dinitrophenyl.hydrazone (ADNPH) was eluted and separated by a reversed-phase column, C-18, under isocratic conditions with the mobile phase containing a binary mixture of methanol/LiCl(aq) at a concentration of 1.0 x 10(-3) M (80:20 v/v) and a flow rate of 1.0 mL min(-1). The optimum condition for the electrochemical detection of ADNPH was +1.0 V vs. Ag/AgCl as a reference electrode. The proposed method was simple, rapid (analysis time 7 min) and sensitive (detection limit 3.80 mu g L-1) at a signal-to-noise ratio of 3:1. It was also highly selective and reproducible [standard deviation 8.2% +/- 0.36 (n = 5)]. The analytical curve of ADNPH was linear over the range of 3-300 mg L-1 per injection (20 mu L), and the analytical recovery was > 99%.

Determination of aldehydes and ketones in fuel ethanol by high-performance liquid chromatography with electrochemical detection

A new methodology was developed for analysis of aldehydes and ketones in fuel ethanol by high-performance liquid chromatography (HPLC) coupled to electrochemical detection. The electrochemical oxidation of 5-hydroxymetkylfurfural, 2-furfuraldehyde, butyraldehyde, acetone and methyl ethyl ketone derivatized with 2,4-dinitrophenylhydrazine (DNPH) at glassy carbon electrode present a well defined wave at +0.94 V; +0.99 V; +1.29 V; +1.15 V and +1.18 V, respectively which are the basis for its determination on electrochemical defector. The carbonyl compounds derivatized were separated by a reverse-phase column under isocratic conditions with a mobile phase containing a binary mixture of methanol /LiClO4(aq) at a concentration of 1.0 x 10(-3) mol L-1 (80:20 v/v) and a flow-rate of 1.1 mL min(-1). The optimum potential for the electrochemical detection of aldehydes-DNPH and ketones-DNPH was +1.0 V vs. Ag/AgCl. The analytical curve of aldehydes-DNPH and ketones-DNPH presented linearity over the range 5.0 to 400.0 ng mL(-1), with detection limits of 1.7 to 2.0 ng mL(-1) and quantification limits from 5.0 to 6.2 ng mL(-1), using injection volume of 20 mu L. The proposed methodology was simple, low time-consuming (15 min/analysis) and presented analytical recovery higher than 95%.

Pharmacokinetic Study of Nobiletin and Tangeretin in Rat Serum by High-Performance Liquid Chromatography-Electrospray Ionization-Mass Spectrometry

Nobiletin (NOB) and tangeretin (TAN), two of the main polymethoxylated flavones (PMFs) in citrus, influence a number of key biological pathways in mammalian cells. Although the impacts of NOB and TAN on glucose homeostasis and cholesterol regulation have been investigated in human clinical trials, much information is still lacking about the metabolism and oral bioavailability of these compounds in animals. In this study, NOB and TAN were administered to rats by gavage and intraperitoneal (ip) injection, and the blood serum concentrations of these compounds and their main metabolites were monitored by high-performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS). In addition to the administered compounds, two metabolites of TAN and eight metabolites of NOB were detected and measured over 24 h. With identical oral doses, nearly 10-fold higher absorption of NOB occurred compared to TAN. For both compounds, maximum levels of glucuronidated metabolites occurred in the blood serum at later time points (similar to 5-8 h) compared to the earlier T(max) a values for NOB and TAN. In most cases the glucuronides occurred at substantially higher concentrations than the aglycone metabolites. Low levels of NOB and TAN and their metabolites were detectable in rat blood serum even at 24 h after treatment.