A single step extraction-cleanup procedure using porous membrane-protected micro-solid phase extraction (μ-SPE) in conjunction with liquid chromatography–tandem mass spectrometry for the extraction and determination of aflatoxins (AFs) B1, B2, G1 and G2 from food was successfully developed. After the extraction, AFs were desorbed from the μ-SPE device by ultrasonication using acetonitrile. The optimum extraction conditions were: sorbent material, C8; sorbent mass, 20 mg; extraction time, 90 min; stirring speed, 1000 rpm; sample volume, 10 mL; desorption solvent, acetonitrile; solvent volume, 350 μL and ultrasonication period, 25 min without salt addition. Under the optimum conditions, enrichment factor of 11, 9, 9 and 10 for AFG2, AFG1, AFB2 and AFB1, respectively were achieved. Good linearity and correlation coefficient was obtained over the concentration range of 0.4–50 ng g−1 (r2 0.9988–0.9999 …
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
... Show MoreA simple, environmental friendly and selective sample preparation technique employing porous membrane protected micro-solid phase extraction (μ-SPE) loaded with molecularly imprinted polymer (MIP) for the determination of ochratoxin A (OTA) is described. After the extraction, the analyte was desorbed using ultrasonication and was analyzed using high performance liquid chromatography. Under the optimized conditions, the detection limits of OTA for coffee, grape juice and urine were 0.06 ng g−1, 0.02 and 0.02 ng mL−1, respectively while the quantification limits were 0.19 ng g−1, 0.06 and 0.08 ng mL−1, respectively. The recoveries of OTA from coffee spiked at 1, 25 and 50 ng g−1, grape juice and urine samples at 1, 25 and 50 ng mL
... Show MoreThis study was done to evaluate a new technique to determine the presence of methamphetamine in the hair using nano bentonite-based adsorbent as the filler of extraction column. The state of the art of this study was based on the presence of silica in the nano bentonite that was assumed can interact with methamphetamine. The hair used was treated using methanol to extract the presence of methamphetamine, then it was continued by sonicating the hair sample. Qualitative analysis using Marquish reagent was performed to confirm the presence of methamphetamine in the isolate.The hair sample that has been taken in a different period confirmed that this current developing method can be used to analyzed methamphetamine. This m
... Show MoreThis work reports the development of an analytical method for the simultaneous analysis of three fluoroquinolones; ciprofloxacin (CIP), norfloxacin (NOR) and ofloxacin (OFL) in soil matrix. The proposed method was performed by using microwave-assisted extraction (MAE), solid-phase extraction (SPE) for samples purification, and finally the pre-concentrated samples were analyzed by HPLC detector. In this study, various organic solvents were tested to extract the test compounds, and the extraction performance was evaluated by testing various parameters including extraction solvent, solvent volume, extraction time, temperature and number of the extraction cycles. The current method showed a good linearity over the concentration ranging from
... 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 MoreAbstract :In this study, amygdaline in Iraqi plant seeds was extracted and isolated from their seeds matrix using reflux procedure and subsequently identified and determined by high performance liquid chromatography (HPLC) on reversed phase column of LC-18 (150mm x 4.6mm, 5?m )with actonitrile :water ( 50 : 50 ) as mobile phase at flow rate of ( 0.5 mL/min ) and detection at wavelength of 215 nm.The experimental results indicated that the linearity of calibration is in the range of 1.0-30.0 mg L-1amygdaline with the correlation coefficient of 0.9949. The limit of detection (LOD) and limit of quantitation (LOQ) for amygdaline were of 0.88 and 2.93 mg L-1 in standard pure sample. The mean recovery percent is 97.34±0.58 at 95% confidence inte
... Show MoreA simple and rapid high performance liquid chromatographic with fluorescence detection method for the determination of the aflatoxin B1, B2, G1 and G2 in peanuts, rice and chilli was developed. The sample was extracted using acetonitrile:water (90:10, v/v%) and then purified by using ISOLUTE multimode solid phase extraction. After the pre-column derivatisation, the analytes were separated within 3.7 min using Chromolith performance RP-18e (100–4.6 mm) monolithic column. To assess the possible effects of endogenous components in the food items, matrix-matched calibration was used for the quantification and validation. The recoveries of aflatoxins that were spiked into food samples were 86.38–104.5% and RSDs were <4.4%. The method was
... Show MoreMany studied were conducted to evaluate the antihepatotoxic and antioxidant activities of Silybum marianum and proved these actions. The Naturally grown seed in Iraqi-Kurdistan Region also were studied for its chemical contents and biological activities. Vegetable oils occur in various plant parts mainly concentrated in the seeds.
In this study comparison was made between the fatty acid patterns of two plant seeds, Silybum marianum and Nigella sativa. Seed sample of Silybum marianum and Nigella sativa were exposed for extraction and isolation of the fatty acid contents using two different solvents (petroleum ether and n-hexane) at 60-80oC using soxhlet apparatus and the oily extract
... Show MoreThe analysis of Iraqi light oil (light naphtha) by capillary gas chromatography- mass spectrometry (GC-MS) was performed by the injection of whole naphtha sample without use of solvents. Qualitative analysis and the identification of the hydrocarbon constituents of light naphtha was performed and comparison had been done with American light oil (light naphtha). The obtained results showed a major difference between the two-light naphtha.
new, simple and fast solid-phase extraction method for separation and preconcentration of trace theophylline in aqueous solutions was developed using magnetite nanoparticles (MIONPs) coated with aluminium oxide (AMIONPs) and modified with palmitate (P) as an extractor (P@AMIONPs). It has shown that the developed method has a fast absorbent rate of the theophylline at room temperature. The parameters that affect the absorbent of theophylline in the aqueous solutions have been investigated such as the amount of magnetite nanoparticle, pH, standing time and the volume, concentration of desorption solution. The linear range, limit of quantification (LOQ) and limit of detection (LOD) for the determination of theophylline were 0.05-2.450 μg mL-
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