Otimização e validação de método multirresíduo para determinação de sulfonamidas em camarão cultivado por cromatografia líquida de alta eficiência com detecção por UV

This work reports the optimization and method validation for sulfonamides (sulfamethazine, sulfaquinoxaline, sulfadimethoxine and sulfathiazole) in shrimp muscle using HPLC-UV. The sulfonamides were extracted with acetonitrile and acetic acid, and the extract cleaned up with a Strata SCX SPE cartridge prior to analysis. The method presented linearity in the range of 20-120 µg kg-1, good linear correlation (r > 0.99), and limits of quantification in the range of 4.7-20.2 µg kg-1. The recovery for shrimp muscles spiked with 50-150 µg kg-1 ranged from 63.2-108.0%. Precision and accuracy analysis showed acceptable relative standard deviation. Commercial shrimps were analyzed and sulfonamides don't were found above of the method limit of quantification.

Isolation and quantitative HPLC-PDA analysis of lupeol in phytopharmaceutical intermediate products from Vernonanthura ferruginea (Less.) H. Rob.

Prior to obtain a standardized dried extract from V. ferruginea, lupeol was first time isolated from leaves and used as chemical maker. An analytical method using HPLC-PDA for lupeol determination in V. ferruginea intermediate products was developed using a C8 reverse-phase column, acetonitrile-acetic acid (99.99:0.01, v/v) as mobile phase at 0.8 mL min-1, oven temperature at 23-25 ºC, sample injection volume at 30 µL and detection at 210 nm. The method presented linearity from 10 to 160 µg mL-1, accuracy, precision, robustness and suitable sensitivity proving to be a useful tool to the obtainment process of lupeol standardized dried extracts of V. ferruginea.

Flavonoids and other bioactive phenolics isolated from Cenostigma macrophyllum (Leguminosae)

This work describes the phytochemical study of stem bark and leaves of Cenostigma macrophyllum Tul. (Leguminosae). Through usual chromatographic techniques were isolated bergenin as the primary compound of the stem bark of and from the leaves gallic acid, methyl gallate, ellagic acid, quercetin, quercetin-3-O-β-D-glucopyranoside, quercetin-3-O-(6"-O-galloyl)-β-D-glucopyranoside (tellimoside), quercetin-3-O-(6"-O-E-p-coumaroyl)-β-D-glucopyranoside (helichrysroside), agathisflavone and vitexin were obtained. The isolates were identified by spectroscopic data analysis, and bergenin showed dose-related antinociception when assessed in acetic acid-induced writhing in mice.

Nanocompósitos ternários de amido termoplástico e poli(Butadieno maleatado)

Liquid polybutadiene (PBLH) was modified with maleic anhydride (MA). The material (PBLHM) was characterized and used to prepare hybrid materials by blending with glycerol-plasticized cassava starch (TPS) and an organophilic clay at 5 wt% content. Processing was performed by extrusion under mild conditions and led to TPS/PBLHM/clay hybrids, at 95/5 to 85/15 TPS/PBLHM compositions, which were characterized by contact angle measurements, X-ray diffraction and mechanical analysis. The results revealed a reduction in the hydrophilicity and the reinforcement of the hybrid materials. Biodegradability tests showed that the addition of clay and of PBLHM led to materials with high biodegradability.

Development and validation of a High Performance Liquid Chromatographic method for determination of etoposide in biodegradable polymeric implants

A method using HPLC-UV was developed and validated for the determination of etoposide incorporated into polycaprolactone implants. The method was carried out in isocratic mode using a C18 column (250 x 4.6 mm; 5 µm), at 25 ºC, with acetonitrile and acetic acid 4% (70:30) as mobile phase, a flow rate of 2 mL/min, and UV detection at 285 nm. The method was linear (r² > 0.99) over the range of 5 to 65 µg/mL, precise (RSD < 5%), accurate (recovery of 98.7%), robust, selective regarding excipient of the sample, and had a quantitation limit equal to 1.76 µg/mL. The validated method can be successfully employed for routine quality control analyses.

Método QuEChERS para determinação de ocratoxina a e citrinina em arroz e farelo de arroz

The present study was carried out to establish the optimal conditions for performing ochratoxin A (OTA) and citrinin (CIT) extraction using the QuEChERS method in rice. Employing the factorial experimental design, variables that significantly influenced the extraction stages were determined. The following variables were analyzed: addition of water, acidification of acetonitrile with glacial acetic acid, as well as amounts of magnesium sulfate, sodium acetate, sodium citrate and diatomaceous earth. The best combining procedure resulted in a predictive model using more water and less diatomaceous earth. Recoveries of CIT and OTA were 78-105%.

A fração volátil das aguardentes de cana produzidas no Brasil

The volatile fraction of sugar cane spirits plays a key role in the quality and acceptance of these beverages. The composition of this fraction is dependent on the way sugar cane collection, fermentation, distillation and aging are carried out. The materials used in these processes strongly influence chemical composition. Acetic acid, acetaldehyde, ethyl acetate, ethanol, 2.3-butanedione, n-propanol, 3-methyl-buthanol and isobuthanol were the major volatiles in spirits. Dimethyl sulfide and n-propanol impaired beverage flavor. Ethyl octanoate, 1.1-diethoxy-ethane, 2-phenylethanol and 3-methyl-butanol were important aroma contributors. Ageing allows the extraction of flavor-active components (e.g., phenolic compounds) from wood.

Implicações químicas na sistemática e filogenia de Bignoniaceae

Our solemn homage to the great Master Otto R. Gottlieb who knew how to teach the mystery of evolutionary relationships between chemistry and its natural sources. The micromolecular chemical study of the family Bignoniaceae shows a profile predominantly characterized by the occurrence of metabolites derived from acetic acid biosynthetic pathways such as terpenoids, quinones, flavonoids and special aromatic derivatives. Analysis of different chemosystematic parameters for the metabolite data collected, provided valuable information for the systematic characterization of the Bignoniaceae family within the Angiosperm derived taxa.

Ácidos orgânicos de baixa massa molar em solos e materiais orgânicos

Determination of organic acids in soils and organic materials is important due to the important role they play in improving the soil's physical, chemical and microbiological conditions. This study identified and quantified low molecular weight organic acids (LMWOA) in soils (dystroferric Red Latosol, dystrophic Red-Yellow Latosol and Quartzarenic Neosol) and organic materials (cow, pig, chicken, quail and horse manures, sawdust, coconut fiber, pine bark, coffee husks, biochar, organic substrate, sewage sludges 1 and 2, garbage compost, pig slurry compost). The following acids were identified: acetic, citric, D-malic, formic, fumaric, maleic, malonic, oxalic, quinic, shikimic, succinic and tartaric.

Registrador portátil de odorantes basado en la modulación de temperatura de un sensor mos comercial

A simple, portable and low-cost system for odor detection was developed using a single MOS commercial sensor and a microcontroller. The temperature modulation technique was implemented applying a DC signal pulse to the sensor heater by a bipolar transistor. Two odorant profiles, ethanol and acetic acid vapors, were obtained and distinguished based on their amplitude versus time responses. Response for acetic acid was not reported by the sensor manufacturer. An ethanol vapor calibration curve was also obtained. Experimental data showed a potential behavior according to the theoretical equation of the MOS sensors. Values of logK=0.457 and α=-0.213 for a 95% confidence level were obtained.

Um reator fotoquímico barato e eficiente para experimentos de química

In this work, we present an efficient and inexpensive device for undergraduate chemistry classes aimed at teaching and learning the photolytic synthesis concepts. A photochemical reactor was tested for the synthesis of the organometallic compound enneacarbonyldiiron from iron pentacarbonyl in acetic acid, and its formation evidenced by FTIR analysis. Although similar devices have been described in other studies, none of these offered the simplicity, low cost, class-compatible reaction times and good yields afforded by the procedure reported herein.

MÉTODO DE SÍNTESE DE AZIDAS AROMÁTICAS USANDO VINAGRE

The present paper describes a simple and low-cost procedure for preparation of aryl azides from anilines using vinegar as an unusual solvent/reagent. We observed the sequence of diazotation followed by diazo displacement with sodium azide can be carried out in aqueous solution of acetic acid

Voimalaitoksen palamisilman esilämmittimen sisäpuolisen korroosion hallinta pinta-aktiivisten amiinien avulla

Useat voimalaitokset käyttävät hiiliteräksistä valmistettuja palamisilman esilämmittimiä, joissa höyrykattilan palamisilmaa lämmitetään matalapainehöyryllä. Joissakin tapauksissa esilämmittimet ovat kärsineet sisäpuolisen korroosion aiheuttamista putkirikoista. Tämän työn tavoitteena oli selvittää korroosiovaurioiden aiheuttajat ja tarkastella eri keinoja uusien korroosiovaurioiden ehkäisemiseksi. Keskeisimpänä uusien vaurioiden ehkäisykeinona tarkastellaan pinta-aktiivisia amiineja sisältäviä höyrykattilan jälkiannostelukemikaaliseoksia, joista tarkemman tarkastelun kohteena on kaupallinen Helamin 90 H Turb- kemikaaliseos. Pääasialliseksi korroosion aiheuttajaksi on usein epäilty höyryn sisältämää hiilidioksidia. Uusimpien näkemysten mukaan orgaaniset hapot, pääasiassa etikka- ja muurahaishappo ovat kuitenkin hiilidioksidia voimakkaampia korroosion aiheuttajia ilmanesilämmittimissä. Orgaaniset hapot väkevöityvät höyryn lauhtumisen alkaessa muodostuviin lauhdepisaroihin ja alentavat pH-tasoa radikaalisti. pH-tason aleneminen nopeuttaa metallipintoja suojaavan magnetiitin liukenemista ja vaikeuttaa myös sen uusiutumista. Orgaanisia happoja ja hiilidioksidia muodostuu orgaanisten aineiden osittaisessa hajoamisessa höyrykattilan vesi-höyrypiirissä. Pääasialliset orgaanisten aineiden lähteet ovat lisäveden mukana kattilaan kulkeutuva luonnon orgaaninen aines ja käytetyt orgaaniset jälkiannostelukemikaalit. Orgaanisten aineiden kuormaa voidaan pienentää parantamalla lisäveden valmistusprosessin orgaanisten aineiden erotustehokkuutta esimerkiksi käänteisosmoosilla. Mikäli lisäveden laadun parantaminen ei ole järkevästi toteutettavissa, voidaan orgaanisten jälkiannostelukemikaalien oikeanlaisella käytöllä neutraloida orgaanisten happojen vaikutus ilmanesilämmittimissä. Tehokkaimmaksi korroosion hillitsijäksi suoritettujen mittausten perusteella osoittautuivat kemikaaliseokset, jotka sisältävät alkaloivien amiinien lisäksi kalvoa muodostavaa pinta-aktiivista amiinia.

Chiral separations of mandelic acid by HPLC using molecularly imprinted polymers

Styrene is used in a variety of chemical industries. Environmental and occupational exposures to styrene occur predominantly through inhalation. The major metabolite of styrene is present in two enantiomeric forms, chiral R- and S- hydroxy-1-phenyl-acetic acid (R-and S-mandelic acid, MA). Thus, the concentration of MA, particularly of its enantiomers, has been used in urine tests to determine whether workers have been exposed to styrene. This study describes a method of analyzing mandelic acid using molecular imprinting techniques and HPLC detection to perform the separation of diastereoisomers of mandelic acid. The molecularly imprinted polymer (MIP) was prepared by non-covalent molecular imprinting using (+) MA, (-) MA or (+) phenylalanine, (-) phenylalanine as templates. Methacrylic acid (MAA) and ethylene glycol dimethacrylate (EGDMA) were copolymerized in the presence of the template molecules. The bulk polymerization was carried out at 4ºC under UV radiation. The resulting MIP was grounded into 25~44¼m particles, which were slurry packed into analytical columns. After the template molecules were removed, the MIP-packed columns were found to be effective for the chromatographic resolution of (±)-mandelic acid. This method is simpler and more convenient than other chromatographic methods.

Methylene blue adsorption onto modified lignin from sugar cane bagasse

The adsorption kinetics and equilibrium of methylene blue (MB) onto reticulated formic lignin (RFL) from sugar cane bagasse was studied. The adsorption process is pH, temperature and ionic strength (µ) dependent and obeys the Langmuir model. Conditions for higher adsorption rate and capacity were determined. The faster adsorption (12 hours) and higher adsorption capacity (34.20 mg.g-1) were observed at pH = 5.8 (acetic acid-sodium acetate aqueous buffer), 50 ºC and 0.1 ionic strength. Under temperature (50 ºC) control and occasional mechanical stirring it took from 1 to 10 days to reach the equilibrium.