A rapid high performance liquid chromatography method for the determination of sphinganine (Sa) and sphingosine (So) in urine samples by employing a silica-based monolithic column is described. The samples were first extracted using ethyl acetate and derivatized using ortho-phthaldialdehyde in the presence of 2-mercaptoethanol. C20 sphinganine was used as internal standard. Under the optimized conditions, separation was achieved using a mixture of methanol:water (93:7, v/v), column temperature at 30°C, flow rate of 1 mL min−1, and an injection volume of 10 μL. Good linearity was obtained for Sa and So over the concentration range 20–500 ng mL−1(correlation coefficients ≥0.9978). The detection limits were 0.45 ng mL−1 for Sa and 1.60 n g mL−1 for So in male urine; in female urine the values were 0.85 ng mL−1 and 2.62 ng mL−1 for Sa and So, respectively. Recoveries for spiked urine samples ranged from 98.6 to 108.2% for Sa and 99.9 to 104.0% for So. A marked reduction in separation time (less than 6 min) was found compared to approximately 14 min by using a conventional C18 particle column. Twenty-two urine samples from the healthy donors and seven samples from the liver cancer patients were analyzed using the method.
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
... Show MoreIn the present study twenty samples of human urine were taken
from healthy male and female with different of: ages, occupation and
place of residence. These samples were collected from the hospital to
measure the concentration of radon gas in human urine by using one
of solid state nuclear track detectors LR-115.
The results obtained of the concentrations of radon in healthy human
urine are varying from 2.12×10-3 Bq.l-1 to 4.42×10-3 Bq.l-1 and
these values are less than the allowed limits 12.3×10-3 Bq.l-1.
The present work investigates the effect of; superficial air velocities of: 1, 3, and 6 cm/s for two types of perforated distributor on hydrodynamic characteristic in a gas-liquid dispersion column of; air-water, and airaqueous-n-propanol solution. Bubble distribution, gas holdup, and power consumption are parameters take in consideration. Experimental work was carried out in perspex column of 8.5 cm inside diameter and 1.5 m height. Two types of bubble generator (perforated plate) were fixed at the bottom of the column; plate A (99 holes of 0.5 mm diameter and free area of 0.34%), plate B (20 holes of 1.5 mm diameter and free area of 0.62%). Photographic technique was used to measure the bubble parameters. The experimental results were
... Show MoreA rapid high sensitive and inexpensive economic method has been developed for the Determination of phenoxazine by using molecular spectrophotometry. The method is based on the oxidation of phenoxazine by potassium (meta)periodate in acidic medium. The oxidation conditions were selected to enhance the sensitivity and the stability of the pink colored species which shows an absorption maximum at 530 nm. The Beer’s law was obeyed for phenoxazine concentration range from 1 to 6 µg mL-1 with 0.003 µg mL-1 detection limit and provided variation coefficients between 0.4 to 1.7 %. This method was successfully applied for the determination of phenoxazine in aqueous samples
Background:Amino acid disorders are a major group of inborn error metabolism (IEM) with variable clinical presentation; its diagnosis constitutes a real challenge in a community with high consanguinity rate and no systematic newborn screening.
Objectives: to provide data about amino acid disorders detected in high-risk Iraqi children by using quantitative amino acid fluorescent high performance liquid chromatography (HPLC) analysis.
Type of the study: Cross-sectional study.
Methods: a descriptive cross sectional study from 1st February to 1st December 2014, at Neurological ward and clinic of the Children Welfare teaching Hospital, in Baghdad - Ira
... Show MoreA reversed-phase HPLC method with fluorescence detection for the determination of the aflatoxins B1, B2, G1 and G2 in 42 animal feeds, comprising corn (16), soya bean meal (8), mixed meal (13), sunflower, wheat, canola, palm kernel, copra meals (1 each) was carried out. The samples were first extracted using acetonitrile:water (9:1), and was further cleaned-up using a multifunctional column. Optimum conditions for the extraction and chromatographic separation were investigated. By adopting an isocratic chromatographic system using a mobile phase comprising acetonitrile:methanol:water (8:27:65, v/v/v), the separation of the four aflatoxins was possible within 30 min. Recoveries for aflatoxins B1, B2, G1 and G2 were 98 ± 0.7%, 95 ± 1.0%, 94
... Show MoreA hydrophilic interaction chromatography has been investigated to separate 2-deoxycytidine chosen for nucleoside. A small molecule with specific features for human serum samples was 2-deoxycytidine tested. 2-deoxycytidine has been applied to self-made stationary hydrophilic phases (ZIC1 and ZIC5). The deoxycytidine (dCD) retention was investigated with varying concentrations of sodium acetate buffer, acetonitrile%, and pH. The results confirmed the hydrophilicity of 2-deoxycytidine. The exchanger retention mechanism was studied taking into account 2-deoxycytidine used for describing the interaction of hydrophilic and cation. For both ZIC1 and ZIC5 exchangers, we described and discussed the influence of chromatographic conditions (co
... 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
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