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The present study describes a simple and facile precipitation polymerization technique. For the synthesis of Cd2+ion-imprinted polymer for the selective detoxification of toxic Cd2+ ions from the aqueous samples. The resultant Cd2+-imprinted polymer was characterized by the EDX, SEM, and FTIR. Different parameters were optimized during the adsorption study to achieve the maximum adsorption capability i.e. pH, equilibrium time, temperature shaking speed, and adsorbent dose. The maximum adsorption capacity of Cd2+ion-imprinted polymer was 62.9 mg. g−1 at pH 6. The kinetic study was best defined by pseudo-second-order, while the Langmuir isotherm model well fitted to present data. Good linearity was achieved in (10–100 μg. L−1) concentration range with LOD 0.88 μg. L−1 and LOQ 2.95 μg. L−1. The relative selective factor (K’) of Cd2+-ion and interfering ions was greater than 1 due to the imprinting effect. The developed method was validated by the spiking addition method and obtained good results in accordance with spiking values in real samples. The synthesized ion-imprinted polymer shown higher adsorption capacity than previously reported methods for the selective removal of Cd2+-ions from aqueous samples.

The extracted oils from four apple seed varieties (Royal Gala, Red Delicious, Pyrus Malus and Golden Delicious) from Pakistan were investigated for their fatty acid profiles and lipid biactives by GC-MS. The oil contents in the seeds of the apple varieties ranged from 26.8-28.7%. The results revealed that linoleic acid (40.5-49.6%) was the main fatty acid in the Royal Gala, Red Delicious and Pyrus Malus seeds, and oleic acid (38.7-45.5%) was the main fatty acid in the Golden Delicious seeds. Palmitic acid (6.1-7.4%) and stearic acid (2.0-3.1%) were the dominant saturated fatty acids, besides the small amount of palmitoleic, heptadecanoic, linolenic, archidic, eicosanoic, and behenicacids. Sterols, tocopherols, hydrocarbons and some other minor components were also identified from the unsaponifiable lipid fraction. The variation among the results of both fatty acids and lipid bioactives for the four different varieties was assessed by principal component analysis, discriminant analysis and cluster analyses. The results conclude that both oil fractions could be applied as a useful tool to discriminate among the apple seed varieties.Se ha estudiado el perfil de ácidos grasos y lípidos biactivos mediante GC-MS del aceite extraído de semillas de cuatro variedades de manzanas de Pakistán (Royal Gala, Red Delicious, Pyrus Malus y Golden Delicious). El contenido de aceite en las semillas de las variedades de manzanas estudiadas oscilaron desde 26,8 hasta 28,7%. Los resultados mostraron que el ácido linoleico (40.5-49.6%) fue el principal ácido graso de las semillas de las variedades Royal Gala, Red Delicious y Pyrus Malus, y el ácido oleico (38,7-45,5%) fue el principal ácido graso de Golden Delicious. Los ácidos palmítico (6.1-7.4%) y esteárico (2,0-3,1%) fueron los ácidos grasos saturados predominantes, las semillas contenían también pequeñas cantidades de palmitoleico, heptadecanoico, linolénico, araquídico, eicosanoico, y behénico. Esteroles, tocoferoles, hidrocarburos, y otros componentes menores también fueron identificados a partir de la fracción insaponificable. La variación de los resultados de ambos, ácidos grasos y lípidos bioactivos, de cuatro variedades diferentes se evaluó mediante análisis de componentes principales, análisis discriminante y análisis de cluster. Los resultados concluyen que las dos fracciones lipídicas de semillas de manzanas podrían aplicarse como una herramienta útil para distinguir variedades.

Fourier transform infrared spectroscopy (FTIR) based methods for the determination of two anti-diabetic drugs, i.e., metformin HCl and glimepiride in tablet formulation are described. The methods involve the use of carefully prepared KBr discs with standards and samples of metformin HCl and glimepiride. FTIR spectra were acquired in the mid IR region. Extraction and pre concentration procedures were totally avoided. For quantification of metformin HCl, a prominent IR band appearing at fixed location height 3173 cm-1 with two point baseline between 3550-2850 cm-1 and for glimepiride IR band at fixed location height 1708 cm-1 with two point baseline between 1800-1600 cm-1 were selected for Beer's law calibrations. For metformin HCl, calibrations were developed using standards in the range between 0.300 mg to 3.100 mg whereas for glimepiride, calibrations were developed using standards in the range between 0.400 mg to 2.450 mg. Accuracy and reproducibility of proposed methods were evaluated and found to be satisfactory with excellent regression coefficients, acceptable recoveries and low standard deviations. The FTIR methods were successfully applied for the quantification of pharmaceutical tablets formulation containing metformin HCl and glimepiride as active substances and the results were found to be comparable with the quoted values. Métodos baseados em espectroscopia de infravermelho com transformada de Fourier (FTIR) para a determinação de duas drogas anti-diabetes, i.e., metformina HCl e glimepirida em formulações de comprimidos, são descritos. Os métodos envolvem o uso de discos de KBr, cautelosamente preparados, com padrões e amostras de metformina HCl e glimepirida. Espectros de FTIR foram adquiridos na região de infravermelho média. A extração e pré-concentração foram evitadas. Para a quantificação da metformina HCl, uma banda de IR proeminente, com localização fixa em 3173 cm-1 com dois pontos na linha base, entre 3550-2850 cm-1 e para a glimepirida, uma banda com localização fixa em 1708 cm-1, com dois pontos na linha base, entre 1800-1600 cm-1 foram selecionados para a calibração usando a lei de Beer. Para a metformina HCl, desenvolveu-se calibrações usando padrões na faixa entre 0,300 mg a 3,100 mg, enquanto que para a glimepirida, as calibrações foram desenvolvidas usando padrões na faixa entre 0,400 a 2,450 mg. Precisão e reprodutibilidade dos métodos propostos foram avaliadas e classificadas como satisfatórias com coeficientes de regressão excelentes, recuperação aceitável e baixos desvios do padrão. Os métodos de FTIR foram aplicados com sucesso na quantificação de formulações de fármacos contendo metformina HCl e glimepirida como substâncias ativas e os resultados comparáveis aos valores citados.

An atomic absorption spectrophotometric method has been devised for the rapid determination of trace metals, found in several vegetable oils and fats. Samples were prepared using an ultrasonically assisted acid-extractive technique. The parameters of the analysis were optimized to improve the recovery of metals from the oil matrixes at an ultra trace level within the least possible time. The use of ultrasonic intensification, followed by centrifugation for phase separation reduced the conventional acid extraction time from 180 to only 10 minutes. The respective range of recovery of iron, copper, nickel and zinc was found to be 94.6-98.0 %, 93.6-100.4 %, 95.0-97.3 % and 96.0-101.2 % in a soybean oil which was fortified with 0.10, 0.25, 0.50, 0.75, 1.00 μg/gm of each of the metals using the standard addition method. The ranges of recovery of these metals as investigated by the proposed method were also found in close agreement with those of the wet digestion method. Most of the samples of commercial oils and fats were found to be contaminated with notable amounts of iron and nickel ranging from 0.13-2.48 and 0.027-2.38 ppm respectively. The contents of copper and zinc were also high in many brands, ranging from 0.01-0.15 ppm and zinc 0.03- 0.21 ppm respectively, which poses a threat to oil quality and to human health.Se ha establecido un método analítico rápido mediante espectroscopia de absorción atómica para determinar con rapidez trazas metálicos en algunos aceites y grasas. Las muestras se preparan mediante una técnica extractiva que utiliza ultrasonidos. Los parámetros del análisis han sido optimizados para mejorar la recuperación de metales a niveles de ultra-traza en el menor tiempo posible. El uso de ultrasonidos, seguido por centrifugación para la separación de fases, redujo el tiempo convencional de extracción de 180 a 10 min. Los rangos de recuperación de hierro, cobre, níquel y zinc fueron 94.6-98.0 %, 93.6-100.4 %, 95.0-97.3 % y 96.0-101.2 %, respectivamente, cuando se utilizó un aceite de soja fortificado con 0.10, 0.25, 0.50, 0.75, 1.00 μg/gm de cada metal utilizando el método estándar de adición. Los rangos de recuperación de los metales fueron muy similares a los obtenidos mediante el método de digestión húmeda. En la mayor parte de las muestras de aceites y grasas analizadas se encontraron cantidades significativas de hierro y níquel que oscilaron entre 0.13-2.48 ppm y 0.027-2.38 ppm, respectivamente, mientras que los contenidos de cobre y zinc oscilaron entre 0.01-0.15 ppm y 0.03- 0.21 ppm, respectivamente.

The purpose of this study was to develop a rapid, simple and sensitive quantitation method for pseudoephedrine (PSE), paracetamol (PAR) and loratadine (LOR) in plasma and pharmaceuticals using liquid chromatography-tandem mass spectrometry with a monolithic column. Separation was achieved using a gradient composition of methanol-0.1% formic acid at a flow rate of 1.0 mL min-1. Mass spectral transitions were recorded in SRM mode. System validation was evaluated for precision, specificity and linearity. Limit of detection for pseudoephedrine, paracetamol, and loratadine were determined to be 3.14, 1.86 and 1.44 ng mL-1, respectively, allowing easy determination in plasma with % recovery of 93.12 to 101.56%.