RESUMO
The aim of present study was to assess pesticide residues in vegetables in the Hyderabad region of Pakistan. The concentrations of six pesticides were determined by gas chromatography coupled with mass selective detector (GC-MSD) in locally produced vegetables purchased from wholesale markets. A total of 200 samples of eight vegetables viz. cauliflower, green chilli, eggplant, tomato, peas, bitter gourd, spinach and apple gourd were analyzed for pesticide residues. The results indicated that almost all samples were contained pesticides, only 39% contained pesticide residues at or below maximum residue limits (MRLs), and 61% contained pesticide residues above MRLs. From the six analyzed pesticides, carbofuran and chlorpyrifos were found above to MRLs with concentrations ranging from 0.01-0.39 and 0.05-0.96 mg/kg, respectively. The results provided important information on the current pesticide contamination status of some commonly used vegetables and pointed an urgent need to control the use of some excessively applied and potentially persistent pesticides, such as carbofuran and chlorpyrifos.
Assuntos
Monitoramento Ambiental , Resíduos de Praguicidas/análise , Poluentes do Solo/análise , Verduras/química , Capsicum/química , Clorpirifos/análise , Humanos , Solanum lycopersicum/química , Malus/química , Paquistão , Medição de RiscoRESUMO
Reports abound on Lernaea parasitizing the brood stock, fingerlings, and marketable-sized culturable freshwater fish species in various parts of the world. We investigated seven small-scale aquaculture farms and how the prevailing Lernaea is impacting them. Randomly seven fish farms were selected to determine the prevalence percentage of lernaeid ectoparasites. Relevant information of the fishponds to estimate the various aspects such as effects of water source and quality, feed, stocking density, treatment used, and weight and length of fish, concerned with Lernaea infestation and prevalence was gathered. The results indicated that Catla catla (F. Hamilton, 1822) showed highest prevalence (41.7%) among the seven fish species, whereas Oreochromis niloticus showed zero. Other five fish species Ctenopharyngodon idella, Cirrhinus cirrhosis, Cyprinus carpio, Labeo rohita and Hypophthalmichthys molitrix showed 13.2%, 8.1%, 7.7%, 7.4%, 0.9% prevalence, respectively. In Royal Fish Farm 84.3% lernaeid infestation was observed, while no parasite was observed in the Vicent's Chunnian fish farm. The water source, quality, feed, fertilizers, stocking density, water temperature, and potential treatment options displayed varying tendencies among fish farms and prevalence. Depending on the weight and length, the highest prevalence (56.7%, and 66.7%) was observed in 3501-4000 g and 81-90 cm groups. The infestation rate varied in various fish body parts with the dorsal fin the most vulnerable organ and showed 2.3% overall prevalence (while 18.4% contribution within total 12.6% infestation). Out of 147 infected fish samples, 45 were extensively contaminated by Lernaea spread. In conclusion, our findings confirm that Lernaea could pose a considerable threat to marketable fish, and various treatment options should be educated to the farmers to help mitigate the spread and potential losses. Furthermore, Catla catla is more vulnerable to Lernaea infestation (41.7%), so are the fish species being cultured at higher stocking densities.
Assuntos
Carpas , Parasitos , Animais , Pesqueiros , Água Doce , Paquistão/epidemiologia , PrevalênciaRESUMO
A study was conducted to evaluate the natural occurrence of aflatoxins (AFB1, AFB2, AFG1, AFG2) in cotton seeds (n = 110) and cotton seed cake (CSC; n = 110) from Pakistan. All samples were screened by Enzyme-Linked ImmunoSorbent Assay (ELISA). Positive samples were further quantified by IAC-HPLC-FLD. Total contamination frequency and aflatoxins mean levels were 80% and 69 µg/kg in cotton seeds and the corresponding values for cotton seed cake 88% and 89 µg/kg, respectively. Aflatoxin B1was found in all positive samples and co-occurred with AFB2, AFG1, and AFG2. Sixty-four cotton seeds and 71 CSC samples contained aflatoxins levels higher than the ML set for animal feed (20 µg/kg). The results of the present study will help the regulatory authorities to formulate strategies for monitoring aflatoxins in animal feeds.
Assuntos
Aflatoxinas/análise , Ração Animal/análise , Contaminação de Alimentos/análise , Gossypium/química , Sementes/química , Animais , PaquistãoRESUMO
Abstract Reports abound on Lernaea parasitizing the brood stock, fingerlings, and marketable-sized culturable freshwater fish species in various parts of the world. We investigated seven small-scale aquaculture farms and how the prevailing Lernaea is impacting them. Randomly seven fish farms were selected to determine the prevalence percentage of lernaeid ectoparasites. Relevant information of the fishponds to estimate the various aspects such as effects of water source and quality, feed, stocking density, treatment used, and weight and length of fish, concerned with Lernaea infestation and prevalence was gathered. The results indicated that Catla catla (F. Hamilton, 1822) showed highest prevalence (41.7%) among the seven fish species, whereas Oreochromis niloticus showed zero. Other five fish species Ctenopharyngodon idella, Cirrhinus cirrhosis, Cyprinus carpio, Labeo rohita and Hypophthalmichthys molitrix showed 13.2%, 8.1%, 7.7%, 7.4%, 0.9% prevalence, respectively. In Royal Fish Farm 84.3% lernaeid infestation was observed, while no parasite was observed in the Vicents Chunnian fish farm. The water source, quality, feed, fertilizers, stocking density, water temperature, and potential treatment options displayed varying tendencies among fish farms and prevalence. Depending on the weight and length, the highest prevalence (56.7%, and 66.7%) was observed in 3501-4000 g and 81-90 cm groups. The infestation rate varied in various fish body parts with the dorsal fin the most vulnerable organ and showed 2.3% overall prevalence (while 18.4% contribution within total 12.6% infestation). Out of 147 infected fish samples, 45 were extensively contaminated by Lernaea spread. In conclusion, our findings confirm that Lernaea could pose a considerable threat to marketable fish, and various treatment options should be educated to the farmers to help mitigate the spread and potential losses. Furthermore, Catla catla is more vulnerable to Lernaea infestation (41.7%), so are the fish species being cultured at higher stocking densities.
Resumo Abundam os relatórios sobre Lernaea parasitando o estoque de cria, alevinos e espécies de peixes de água doce cultiváveis de tamanho comercial em várias partes do mundo. Investigamos sete fazendas de aquicultura de pequena escala e de que maneira a Lernaea predominante está impactando-as. Aleatoriamente, sete fazendas de peixes foram selecionadas para determinar a porcentagem de prevalência de ectoparasitas de Lernaea. Foram recolhidas informações relevantes sobre os viveiros de peixes para estimar os vários aspectos, tais como efeitos da fonte e qualidade da água, alimentação, densidade de povoamento, tratamento utilizado e peso e comprimento dos peixes, relacionados com a infestação e prevalência de Lernaea. Os resultados indicaram que Catla catla (F. Hamilton, 1822) apresentou maior prevalência (41,7%) entre as sete espécies de peixes, enquanto Oreochromis niloticus apresentou zero. Outras cinco espécies de peixes Ctenopharyngodon idella, Cirrhinus cirrhosis, Cyprinus carpio, Labeo rohita e Hypophthalmichthys molitrix apresentaram 13,2%, 8,1%, 7,7%, 7,4%, 0,9% de prevalência, respectivamente. Em Royal Fish Farm, 84,3% de infestação de Lernaea foi observada, enquanto não se observou nenhum parasita na fazenda de peixes Chunnian de Vicent. A fonte de água, qualidade, ração, fertilizantes, densidade de estocagem, temperatura da água e opções de tratamento potenciais exibiram tendências variadas entre as fazendas de peixes e prevalência. Dependendo do peso e comprimento, a maior prevalência (56,7% e 66,7%) foi observada nos grupos de 3501-4000 g e 81-90 cm. A taxa de infestação variou em várias partes do corpo dos peixes, sendo a nadadeira dorsal o órgão mais vulnerável e apresentou 2,3% de prevalência geral (enquanto 18,4% de contribuição dentro do total de 12,6% de infestação). Das 147 amostras de peixes infectados, 45 estavam amplamente contaminadas pela propagação de Lernaea. Em conclusão, nossos resultados confirmam que Lernaea pode representar uma ameaça considerável para peixes comercializáveis, e várias opções de tratamento devem ser educadas para os agricultores para ajudar a mitigar a propagação e as perdas potenciais. Além disso, Catla catla é mais vulnerável à infestação por Lernaea (41,7%), assim como as espécies de peixes sendo cultivadas em densidades de estocagem mais altas.
RESUMO
Substantive improvement in the sensitivity of the AOAC/AOCS spectral ratioing method for the determination of isolated trans isomers in edible oils was recently achieved by the application of a new spectral reconstitution (SR) technique that facilitates the FTIR analysis of edible oils in the transmission mode. However, the general applicability of the spectral ratioing method is still severely limited by the requirement to know the provenance of the oil to be analyzed and have on hand its trans-free counterpart so that the underlying triacylglycerol absorptions in the trans measurement region (990-945 cm(-1)), henceforth referred to as UAt , may be ratioed out. To eliminate the need for a trans-free reference oil, we have employed two-dimensional (2D) correlation spectroscopy to search for other spectral features that might correlate with and serve to estimate the UAt . The three-dimensional contour maps obtained by 2D correlation analysis of the spectra of 10 trans-free oils of different oil types, recorded using the SR procedure, revealed such correlations in two spectral regions, 1700-1600 and 4500-4300 cm(-1), exhibiting one maximum and two maxima, respectively, with wavenumber coordinates of (968, 4407), (968, 4299), and (968, 1650). The latter two correlations, when optimized, produced excellent linear regression relationships (r>0.95) with the UAt . The spectra of five sets of trielaidin-spiked oils were corrected for the UA t using these relationships, and their trans contents were predicted from the calibration equation generated for the spectral ratioing procedure. Linear regression of predicted versus added trans over the range of 0-1.6% trans, which is below the limit of quantitation of the AOAC/AOCS spectral ratioing method, yielded r=0.88-0.90 with an SD of approximately 0.2% trans. These results indicate that the combination of the SR technique with the UA t correction approach may provide a simple and accurate FTIR method for the analysis of the trans content of fats and oils that would be competitive with GC.
Assuntos
Técnicas de Química Analítica/métodos , Análise de Alimentos/métodos , Óleos de Plantas/análise , Espectrofotometria/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Automação , Calibragem , Isomerismo , Modelos Lineares , Reprodutibilidade dos Testes , Sensibilidade e EspecificidadeRESUMO
Ten margarine brands of Pakistan were analyzed for their fatty acid composition with emphasis on trans fatty acids (TFA) using GC-MS. Saturated, cis-monounsaturated and polyunsaturated fatty acids were present at 24.2-58.1, 5.7-35.4 and 3.8-37.4% of total fatty acids, respectively. Among the saturated fatty acids, palmitic acid (16.9-33.8%) was dominant in all analyzed margarine brands and its higher amount indicates that palm oil was a major contributor in the margarine manufacturing. Among samples tested only one contained a low level of TFA (2.2%) while the rest contained very high amounts of TFA (11.5-34.8%) which clearly shows that hydrogenated oils were used in the formulation of margarines. Fatty acid profiles demonstrated that all samples belong to the hard margarine category containing high amounts of trans and saturated fatty acids which is an alarming issue for the health of consumers.
RESUMO
The present study was undertaken to assess the intramuscular fatty acid composition of different muscles taken from male Pateri (n=15) goats, reared on naturally grown grasses, leaves and pods of Acacia nilotica and crushed cereal, under traditional way of feeding. Goats were slaughtered with an average weight of 68±7kg and age 12±1 month. The samples were taken from longissimus dorsi region (between the 12th and 13th rib) and distal region of semitendinosus muscle. Results of total fat content and fatty acids composition does not show significant (P>0.05) variation among muscles investigated. The fatty acid composition of muscles studied were primarily composed of oleic (31.50-33.38%), followed by palmitic acid (19.84-22.05%) and stearic acid (22.25-24.91%) respectively. Muscle tissue in general contained an average 51.13% of saturated fatty acids and 48.87% of unsaturated fatty acids. The mean conjugated linoleic acid was found 0.41%, 0.43% and 0.47% in ribeye and loin portion of longissimus dorsi muscle and distal region of semitendinosus muscle, respectively.
RESUMO
Plasmonic response of silver nanoparticles (AgNPs) reduced with phenolic compounds were evaluated and correlated with the antioxidant capacities of corresponding phenolic compounds and their relative chemical structures. The reference methods including DPPH (2,2-diphenyl-1-picrylhydrazyl) and ABTS (2,2'-azinobis(3-ethylbenzothiazoline-6-sulfonic acid)) radical scavenging assays were used for the measurement of antioxidant capacity of phenolic compounds which was positively correlated with redox characteristics of these compounds against the formation of AgNPs. It is found that the higher plasmonic response of AgNPs corresponds to the highest antioxidant capacity of phenolic acids, which in turn depends on chemical structures and degree of hydroxylation. The higher degree of hydroxylation in chemical structures of phenolic compounds demonstrated the higher radical scavenging capacity and higher tendency to reduce Ag+ to AgNPs. The influence of reaction time and temperature on reducing efficiency of the tested phenolic compounds is found to be different. Some phenolic compounds such as quercetin, rutin and gallic acid reacted fast (<â¯1.0â¯min) while others were found slow reacting. This study establishes the relationship between the antioxidant capacity of phenolic acids and corresponding optical response by means of plamonics, which can be used as an innovative antioxidant detection assay for samples rich in phenolic compounds.
RESUMO
A simple, rapid, and reproducible method has been developed for the quantitative determination of free fatty acid (FFA) content in lipids extracted from poultry feeds by Fourier transform infrared (FTIR) spectroscopy with the use of a single-bounce attenuated total reflectance (SB-ATR) accessory. An FTIR calibration curve was prepared by gravimetrically adding oleic acid (15-37%) to pure refined, bleached, and deodorized (RBD) canola oil and measuring the area of the COOH absorption band at 1710 cm-1. The oil from each of 12 poultry feed formulations was extracted using conventional Soxhlet extraction, and after evaporation of the solvent, the FFA content was determined by the conventional AOCS titrimetric procedure and by the SB-ATR/FTIR method. The SB-ATR/FTIR FFA predictions were related to those determined by the AOCS titrimetric method by linear regression, producing an R value of 0.999 and a SD of +/-0.28% FFA. Time-course spectra collected as lipids extracted into hexane indicated that a 15 min extraction was adequate to obtain a representative sample for FFA determination, with further extraction resulting in little, if any, change in the proportion of FFA in the lipid extract. Only a small volume of the hexane extract ( approximately 20 mL) yielded sufficient material for the SB-ATR/FTIR analysis. Thus, by shortening the extraction time and taking a small sample so as to reduce solvent removal time, the SB-ATR/FTIR procedure provides a very simple and rapid means of determining the FFA content of poultry feed lipids.
Assuntos
Ração Animal/análise , Ácidos Graxos não Esterificados/análise , Lipídeos/análise , Aves Domésticas , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , AnimaisRESUMO
A study was conducted to evaluate the occurrence of ochratoxin A (OTA) in complete poultry feeds (n=80) and poultry feed ingredients (n=286) from Pakistan. All samples were first analyzed by indirect enzyme linked immunosorbent assay (ELISA), samples with OTA concentrations above the European Union maximum regulatory limit (MRL, 100 µg/kg) were further confirmed by HPLC-FLD. Contamination frequency and mean OTA levels were 31% and 51 µg/kg in feed ingredients, and the corresponding values for complete feeds were 38% and 75 µg/kg. Ten samples of complete poultry feed and 19 samples of feed ingredients contained OTA at levels higher than the MRL. The results of the present study indicate that there is a strong need for a more intense monitoring programs for OTA in poultry feed.
Assuntos
Ração Animal/análise , Contaminação de Alimentos/análise , Ocratoxinas/análise , Animais , Cromatografia Líquida de Alta Pressão , Ensaio de Imunoadsorção Enzimática , Inocuidade dos Alimentos/métodos , Paquistão , Aves DomésticasRESUMO
Transmission Fourier transform infrared (FTIR) spectroscopic method using 100 µm KCl cell was applied for the determination of total polar compounds (TPC), carbonyl value (CV), conjugated diene (CD) and conjugated triene (CT) in canola oil (CLO) during potato chips frying at 180 °C. The calibration models were developed for TPC, CV, CD and CT using partial least square (PLS) chemometric technique. Excellent regression coefficients (R(2)) and root mean square error of prediction values for TPC, CV, CD and CT were found to be 0.999, 0.992, 0.998 and 0.999 and 0.809, 0.690, 1.26 and 0.735, respectively. The developed calibration models were applied on samples of canola oil drawn during potato chips frying process. A linear relationship was obtained between CD and TPC with a good correlation of coefficient (R(2)=0.9816). Results of the study clearly indicated that transmission FTIR-PLS method could be used for quick and precise evaluation of oxidative changes during the frying process without using any organic solvent.
Assuntos
Culinária , Bases de Dados de Compostos Químicos , Ácidos Graxos Monoinsaturados/química , Calibragem , Análise dos Mínimos Quadrados , Oxirredução , Óleo de Brassica napus , Espectroscopia de Infravermelho com Transformada de FourierRESUMO
Radiation dose outside the radiotherapy treatment field can be significant and therefore is of clinical interest in estimating organ doses. In a previous paper we reported the results of measurements made using unmodified radiation fields. We have extended this study to include the effects of wedge filters and blocks. For a given dose on the central axis of a radiation field, wedges can cause a factor of 2 to 4 increase in dose at any point outside the field compared with the dose when no wedge is used. Adding blocks to a treatment field can cause an increase in dose at points outside the field, but the effect is much smaller than the effect of a wedge, and generally less than a factor of 2. From the results of these measurements, doses to selected organs outside the field for specified treatment geometries were estimated, and the potential for reducing these organ doses by additional shielding was assessed.
Assuntos
Monitoramento de Radiação , Radioterapia/instrumentação , Humanos , Matemática , Espalhamento de Radiação , ÁguaRESUMO
Biologically active complexes of cobalt (II) and nickel (II) with thienoyl- and furenoyl-derived Schiff-base ligands having the same metal ion but different anions such as sulfate, nitrate, oxalate and acetate have been prepared and characterized. In order to evaluate the role of anions on their pharmacological properties the synthesized complexes have been screened against bacterial species, Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa and results have been reported.
RESUMO
Two hundred and fifteen broiler poultry feed samples were analysed over the time period of one year for the co-occurrence of aflatoxins and deoxynivalenol (DON). These were determined by GC-MS and ELISA, respectively. LOD values for aflatoxins and DON were 0.5 and 5 µg/kg, respectively. From all investigated 215 poultry feed samples, aflatoxins and DON co-occurred in 100 samples (46%). DON was detected in 114 samples while 100 samples also were positive for aflatoxins. Mean concentrations of positive samples for aflatoxins and DON were 18 and 807 µg/kg, respectively. Twenty-one DON-positive and 42 aflatoxin positive samples were contaminated above the EU maximum legal limits of 1000 µg/kg and 20 µg/kg, respectively. The present study provided useful data on aflatoxin and DON contamination, which may be helpful for future strategies to control contamination and to formulate standards in poultry feeds.
Assuntos
Aflatoxinas/análise , Ração Animal/análise , Contaminação de Alimentos/análise , Aves Domésticas , Tricotecenos/análise , Animais , Ensaio de Imunoadsorção Enzimática , Cromatografia Gasosa-Espectrometria de Massas , Limite de Detecção , PaquistãoRESUMO
Single bounce attenuated total reflectance (SB-ATR) Fourier transform infrared (FTIR) spectroscopy in conjunction with chemometrics was used for accurate determination of free fatty acid (FFA), peroxide value (PV), iodine value (IV), conjugated diene (CD) and conjugated triene (CT) of cottonseed oil (CSO) during potato chips frying. Partial least square (PLS), stepwise multiple linear regression (SMLR), principal component regression (PCR) and simple Beer׳s law (SBL) were applied to develop the calibrations for simultaneous evaluation of five stated parameters of cottonseed oil (CSO) during frying of French frozen potato chips at 170°C. Good regression coefficients (R(2)) were achieved for FFA, PV, IV, CD and CT with value of >0.992 by PLS, SMLR, PCR, and SBL. Root mean square error of prediction (RMSEP) was found to be less than 1.95% for all determinations. Result of the study indicated that SB-ATR FTIR in combination with multivariate chemometrics could be used for accurate and simultaneous determination of different parameters during the frying process without using any toxic organic solvent.
Assuntos
Técnicas de Química Analítica/métodos , Óleo de Sementes de Algodão/química , Análise de Alimentos/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Calibragem , Ácidos Graxos não Esterificados/química , Manipulação de Alimentos , Iodo/química , Análise dos Mínimos Quadrados , Modelos Lineares , Modelos Estatísticos , Análise Multivariada , Peróxidos/química , Solanum tuberosum , Solventes/químicaRESUMO
Melamine is a nitrogenous chemical substance used principally as a starting material for the manufacture of synthetic resins. Due to its very high proportion of nitrogen melamine has been added illegitimately to foods and feeds to increase the measured protein content, which determines the value of the product. These issues prompted private as well as governmental laboratories to develop methods for the analysis of melamine in a wide variety of food products and ingredients. Owing to this fact present study is aimed to use single bounce attenuated total reflectance (SB-ATR) Fourier transform infrared spectroscopy (FTIR) method as an effective rapid tool for the detection and quantification of melamine in milk (liquid and powder). Partial least-squares (PLS) models were established for correlating spectral data to melamine concentration with R(2)>0.99, and RMSEC 0.370. Linear calibration curves were obtained over the calibration range of 25-0.0625%. The LOD and LOQ of the method was 0.00025% (2.5 ppm) and 0.0015% (15 ppm) respectively. Proposed SB-ATR-FTIR method requires little or no sample preparation with an assay time of 1-2 min.
Assuntos
Contaminação de Alimentos/análise , Leite/química , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Triazinas/análise , Animais , BovinosRESUMO
A rapid, reliable and cost effective analytical procedure for the estimation of ibuprofen in pharmaceutical formulations and human urine samples was developed using transmission Fourier Transform Infrared (FT-IR) spectroscopy. For the determination of ibuprofen, a KBr window with 500 µm spacer was used to acquire the FT-IR spectra of standards, pharmaceuticals as well as urine samples. Partial least square (PLS) calibration model was developed based on region from 1807 to 1,461 cm(-1) using ibuprofen standards ranging from 10 to 100 µg ml(-1). The developed model was evaluated by cross-validation to determine standard error of the models such as root mean square error of calibration (RMSEC), root mean square error of cross validation (RMSECV) and root mean square error of prediction (RMSEP). The coefficient of determination (R(2)) achieved was 0.998 with minimum errors in RMSEC, RMSECV and RMSEP with the value of 1.89%, 1.63% and 4.07%, respectively. The method was successfully applied to urine and pharmaceutical samples and obtained good recovery (98-102%).
Assuntos
Anti-Inflamatórios não Esteroides/análise , Anti-Inflamatórios não Esteroides/urina , Ibuprofeno/análise , Ibuprofeno/urina , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Calibragem , Humanos , Análise dos Mínimos Quadrados , Sensibilidade e Especificidade , ComprimidosRESUMO
A quick and reliable analytical method for the quantitative assessment of cefixime in orally administered pharmaceutical formulations is developed by using diamond cell attenuated total reflectance (ATR) Fourier transform infrared (FT-IR) spectroscopy as an easy procedure for quality control laboratories. The standards for calibration were prepared in aqueous medium ranging from 350 to 6000mg/kg. The calibration model was developed based on partial least square (PLS) using finger print region of FT-IR spectrum in the range from 1485 to 887cm(-1). Excellent coefficient of determination (R(2)) was achieved as high as 0.99976 with root mean square error of 44.8 for calibration. The application of diamond cell (smart accessory) ATR FT-IR proves a reliable determination of cefixime in pharmaceutical formulations to assess the quality of the final product.
Assuntos
Cefixima/análise , Preparações Farmacêuticas/química , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Administração Oral , Calibragem , Cefixima/química , Cromatografia Líquida de Alta Pressão , Pós/química , Padrões de Referência , Suspensões/químicaRESUMO
A non-aqueous flow injection method for determining free fatty acid (FFA) content in corn and sunflower oil samples was developed. A single-line manifold system was built by modification of an HPLC for flow injection analysis (FIA). Without pre-treatment, oil samples were injected into a n-propanol solution containing KOH and phenolphthalein (PHP). The main parameters, such as flow rate of carrier phase, length, geometry, inner diameters of the coils and reagent concentration were all optimized. The proposed FIA method was validated for precision, accuracy, linear region, limit of detection (LOD) and limit of quantification (LOQ). The intra- and inter-day measurements of the precision of the method were found to be within the limits of acceptance criteria (RSD < 1%), and were rugged when the method was performed by a different analyst. The linear concentration range was calculated as 0.09-1.50 and 0.07-1.40 FFA% for corn and sunflower oils, correspondingly. The LOD and LOQ were found to be 7.53 × 10(-4)-2.28 × 10(-3) oleic acid % and 7.11 × 10(-4)-2.23 × 10(-3) oleic acid % for corn and sunflower oils, respectively. The results were compared with those obtained by the AOCS (Ca-5a-40) method using statistical t and F tests, and a significant difference was not observed between the methods at a 95% confidence level. The proposed method is suitable for quality control of routine applications due to its simplicity, high sample throughput, and economy of solvents and sample, offering considerable promise as a low cost analytical system that needs minimum human intervention over long periods of time.
Assuntos
Ácidos Graxos não Esterificados/análise , Análise de Injeção de Fluxo/métodos , Óleos de Plantas/química , 1-Propanol/química , Cromatografia Líquida de Alta Pressão/métodos , Hidróxidos/química , Fenolftaleína/química , Compostos de Potássio/química , Controle de Qualidade , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Óleo de GirassolRESUMO
The present study describes synthesis of a new resin through immobilization of p-tert-butylcalix[8]arene onto silica and its application for the removal of azo dyes from aqueous media as well as from textile effluents. The newly synthesized material 4 is characterized by FT-IR spectroscopy, scanning electron microscope (SEM) and thermogravimetric analysis (TGA). Reactive Black-5 (RB-5) and Reactive Red-45 (RR-45) azo dyes were used as sorbate. Batch wise sorption experiments were conducted to optimize various experimental parameters such as the effect of sorbent dosage, electrolyte, pH, dye concentration, and contact time. The optimized pH for the effective removal of RB-5 and RR-45 dyes was 9 and 3, respectively. The increase in material 4 dosage increased the percent sorption. Both Langmuir and Freundlich isotherm models were applied to experimental data and Langmuir isotherm model found to be best fit. The results revealed that material 4 was potentially more effective sorbent for the sorption of selected azo dyes as compared to pure silica and p-tert-butylcalix[8]arene. The field studies also supported the effectiveness of material 4, which could be useful for the removal of both the dyes and also for the normalization of pH, TDS, conductivity and salinity near to the drinking water.