The development of a reversed phase high performance liquid chromatography fluorescence method for the determination of the mycotoxins fumonisin B1 and fumonisin B2 by using silica-based monolithic column is described. The samples were first extracted using acetonitrile:water (50:50, v/v) and purified by using a C18 solid phase extraction-based clean-up column. Then, pre-column derivatization for the analyte using ortho-phthaldialdehyde in the presence of 2-mercaptoethanol was carried out. The developed method involved optimization of mobile phase composition using methanol and phosphate buffer, injection volume, temperature and flow rate. The liquid chromatographic separation was performed using a reversed phase Chromolith® RP-18e column (100 mm × 4.6 mm) at 30 °C and eluted with a mobile phase of a mixture of methanol and phosphate buffer pH 3.35 (78:22, v/v) at a flow rate of 1.0 mL min−1. The fumonisins separation was achieved in about 4 min, compared to approximately 20 min by using a C18 particle-packed column. The fluorescence excitation and emission were at 335 nm and 440 nm, respectively. The limits of detections were 0.01–0.04 μg g−1 fumonisin B1 and fumonisin B2, respectively. Good recoveries were found for spiked samples (0.1, 0.5, 1.5 μg g−1 fumonisins B1 and B2), ranging from 84.0 to 106.0% for fumonisin B1 and from 81.0 to 103.0% for fumonisin B2. Fifty-three samples were analyzed including 39 food and feeds and 14 inoculated corn and rice. Results show that 12.8% of the food and feed samples were contaminated with fumonisin B1 (range, 0.01–0.51 μg g−1) and fumonisin B2 (0.05 μg g−1). The total fumonisins in these samples however, do not exceed the legal limits established by the European Union of 0.8 μg g−1. Of the 14 inoculated samples, 57.1% contained fumonisin B1 (0.16–41.0 μg g−1) and fumonisin B2 (range, 0.22–50.0 μg g−1). Positive confirmation of selected samples was carried out using liquid chromatography–tandem mass spectrometry, using triple quadrupole analyzer and operated in the multiple reaction monitoring mode.
Silver nanoparticles synthesized by different species
A simple, accurate and sensitive spectrophotometric method for the determinaion of epinephrine is described . The method is based on the coordination of Pr (III) with epinephrine at pH 6. Absorbance of the resulting orange yellow complex is measured at 482 nm . A graph of absorbance versus concentrations shows that beer 's low is obeyed over the concentration range (1-50)mg.ml-1 of epinephrine with molar absorpitivity of ( 2.180x103 L.mol-1.cm-1 ), a sandell sensitivity of (0.084 mg.cm-2 ), a relative error of (-2.83%) , a corrolation coffecient (r= 0.9989) and recovery % ( 97.03 ± 0.75 ) depending on the concentration.This method is applied to analyse EP in several commercially available pharmaceutical preparations
... Show MoreBased on the diazotization reaction of 4-aminoacetophenone with sodium nitrite in acid medium to form diazonium salt, which was coupled with Methyldopa to form a violet reddish soluble azo dye with maximum absorbance at 560 nm,a batch procedure had been developed for the estamination of Methyldopa. Under optimum experimental parameters affecting on the development and stability of the colored product, Beer´s law obeyed in the range (0.5-45) ?g.ml-1 with a correlation coefficient (0.9979).The proposed method was successfully applied to the determination of Methyldopa in either pure form and in commercial brands of pharmaceuticals, no interference was observed from common excipients in the formulations. The analytical results obtained by app
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Binary logistic regression model used in data classification and it is the strongest most flexible tool in study cases variable response binary when compared to linear regression. In this research, some classic methods were used to estimate parameters binary logistic regression model, included the maximum likelihood method, minimum chi-square method, weighted least squares, with bayes estimation , to choose the best method of estimation by default values to estimate parameters according two different models of general linear regression models ,and different s
... Show MoreIn high-dimensional semiparametric regression, balancing accuracy and interpretability often requires combining dimension reduction with variable selection. This study intro- duces two novel methods for dimension reduction in additive partial linear models: (i) minimum average variance estimation (MAVE) combined with the adaptive least abso- lute shrinkage and selection operator (MAVE-ALASSO) and (ii) MAVE with smoothly clipped absolute deviation (MAVE-SCAD). These methods leverage the flexibility of MAVE for sufficient dimension reduction while incorporating adaptive penalties to en- sure sparse and interpretable models. The performance of both methods is evaluated through simulations using the mean squared error and variable selection cri
... Show MoreAn update of our research is the first to develop and reform the agricultural sector . and promoting production and productivity of this sector multi-sources , which is the management and beekeeping one source . Been applied to the style of beekeeping mobile promiscuous includes twentieth cell in the Iraqe project of mussiab . in which there exist a variety of crops and trees .
Experiment had proved successful and led to raise the level of npoduction of single Dell of the honey to 49 kg over the previous year and surpassed the average production percell in the province of Babylon , which the amount of 13.945 kg , another
... Show MoreThis study aimed to evaluate the occurrence of microbial contamination in food keeping freezers in some local markets in Baghdad city/ Iraq, as well as the contamination of the hands of workers in markets, and the possibility of contamination caused by the transport of food. 30 samples of snow ice found in food keeping freezers in local markets was randomly collected, and 30 swabs from workers hands were taken from the same markets at the same time. Microbiological examination of ice samples was conducted as well as the hands of workers’swabs, and the bacteria were isolated and diagnosed through microbiological and biochemical tests followed. Microbial test results showed some isolates of bacteria in ice samples obtained from food keep
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