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.
Alhagi maurorum (camel thorn) is a grayish, evergreen, deeply rooting plant that has spiny needle -like branches. In our study, the phytochemical contents of the root ethanoloic extract of A. maurorum were determined by using gas chromatography-mass spectroscopy (GC-MS). Thirty two chemical constituents were identified. We revealed the existence of oxalic acid, anti-2 acetoxyacetaldoxime, sulfone, butyl isopropyl, 2,3-pentanedione, 2-butanone, n,n,o triacetylhydroxylamine. di(1,2,5-oxadiazole)[3,4-b;3,4-e]pyrazine, isobutane,3,4-hexanedione,3-hexanone, pentane, 3-pentanone, 3-butene, 2-thiopheneacetic acid, 2-pyrazoline, 4-hepten-3-onemethylphosphonic acid, butane, propanoic acid, methane, azetidine, heptane, butanoic a
... Show MoreNanoparticle has pulled in expanding consideration with the developing enthusiasm for nanotechnology which hold potential as essential segments for development applications. In the present work, a copper nanoparticle is manufactured as a suspension in distilled water by beating a bulk copper target with laser source (532 nm wavelength, 10 ns pulse duration and 10 Hz repletion rate) via method. UV- visible absorption spectra and AFM analysis has been done to observe the effect of repetition rate for the pulsation of laser. Copper nanoparticles (Cu-NPs) were successfully synthesized with green color. The Cu- NPs have very high purity because the preparation was managed in aqueous media to eliminate ambient contaminations. Absorption
... Show MoreA simple and novel method was developed by combination of dispersive liquid-liquid microextraction with UV spectrophotometry for the preconcentartion and determination of trace amount of malathion. The presented method is based on using a small volume of ethylenechloride as the extraction solvent was dissolved in ethanol as the dispersive solvent, then the binary solution was rapidly injected by a syringe into the water sample containing malathion. The important parameters, such the type and volume of extraction solvent and disperser solvent, the effect of extraction time and rate, the effect of salt addition and reaction conditions were studied. At the optimum conditions, the calibration graph was linear in the range of 2-100 ng mL-1 of ma
... Show MoreThe current work is characterized by simplicity, accuracy and high sensitivity Dispersive liquid - Liquid Micro Extraction (DLLME). The method was developed to determine Telmesartan (TEL) and Irbesartan (IRB) in the standard and pharmaceutical composition. Telmesartan and Irbesartan are separated prior to treatment with Eriochrom black T as a reagent and formation ion pair reaction dye. The analytical results of DLLME method for linearity range (0.2- 6.0) mg /L for both drugs, molar absorptivity were (1.67 × 105- 5.6 × 105) L/ mole. cm, limit of detection were (0.0242and0.0238), Limit of quantification were (0.0821and0.0711), the Distribution coefficient were
... Show MoreModification of gas chromatographic technique for the separation and determination of methyl ethoy silane compounds which were synthesized by the addition of absolute ethanol to methyl chlorosilane compounds have been elaborated experimentally. The addition of absolute dry ethanol to methyl chlorosilane compounds in the presence of a dry stream of nitrogen gas led to sweep out the liberated HCl gas. This method was found to be the suitable method for the preparation of methyl ethoxy silane compounds. The optimum parameter selected after careful and precise studies was between 20 – 30 ml \ min to carrieir gas flow rate, while applied temperatures of detector and injection part were 250 Â
... Show MoreA simple, rapid and environmentally friendly dispersive liquid–liquid microextraction method-based spectrophotometric method for the trace determination of folic acid has been developed. The proposed method is based on the formation of a deep yellow product via reaction of folic acid and 1,2-naphthoquine-4-sulfonate at pH = 9. The formed complex was extracted using a mixture of chloroform and ethanol. Then, the tiny organic droplets were measured at λ = 520 nm. At the optimum conditions, linearity was ranged from 0.05 to 1.5 μg/mL for the standard and samples, with a linear correlation coefficient of 0.9996. The detection limits were 0.02, 0.027, 0.03, 0.02 and 0.04 μg/mL for standard, tablet (5 mg), tablet (1 mg), syrup and fl
... Show MoreA rapid and sensitive method for analysis of amino acid hydrolysates of nigella sativa L seed has been developed using O-phthaldialehyde(OPA ) as a pre-column derivatizing agent. OPA reagents in the presence of mercaptoethanol react rapidly with primary amino acids ( less than 60 sec.) to form isindole derivatives which easily separated with good selectivity on ODS column. Resolution of amino acid derivatives is carried out with a methanol gradient in 0.01 maqueous sodium acetate. pH 7.1 . The quantitation of amino acid derivatives is reproducible within an average relative deviation of + 1.4% the linearity for most amino acids were more than 0.9993 with detection limit of 0.2 ppm. 15 amino acid were detected in the analysis of
... Show MoreA method was developed that offers a rapid, simple and accurate technique for the determination of chlorophenols at trace levels in aqueous samples with very limited volumes of organic solvents. These compounds were acetylated, then preliminarily extracted with n-hexane. The enriched chlorophenols were directly analyzed using gas chromatography with an electron-capture detector. The detection limits were in the range of 0.001–0.005 mg/L, except for 2-chlorophenol, which was always above 0.013 mg/L. Relative standard deviation for the spiked water samples ranged from 2.2 to 6.1%, while relative recoveries were in the range of 67.1 to 101.3%.