Search results for "STANDARD"
showing 10 items of 3299 documents
A new derivatization procedure for the determination of cephalexin with 1,2-naphthoquinone 4-sulphonate in pharmaceutical and urine samples using sol…
1998
Abstract The present report shows how to derivatize cephalexin with 1,2-naphthoquinone-4-sulphonate (NQS) into solid-phase extraction cartridges (C18) using UV–visible detection. Optimum conditions for this new procedure are: hydrogen carbonate/carbonate buffer pH=10.5, 5 min reaction time at 25°C and NQS concentration of 7.1×10−3 mol l−1. The accuracy and the precision of the method were tested. The procedure was used to measure cephalexin in pharmaceutical and urine samples. The results obtained were contrasted with those reported by UV-spectrophotometric and HPLC methods for pharmaceutical samples and with HPLC method for urine samples. The H-point standard additions method was used to m…
Determination of trichothecenes in chicken liver using gas chromatography coupled with triple-quadrupole mass spectrometry
2018
Abstract Chicken meat and edible offal are included in a wide number of preparations in the worldwide cuisine. Among the offal, the liver is one of the most consumed in some countries like Egypt since it is rich in proteins and is an economical source of many essential nutrients for humans. Mycotoxins, secondary toxic metabolites produced by fungi, have the potential to enter human food chain not only with cereal consumption but also through edible tissues from animals fed with mycotoxin-contaminated feed. Accordingly, a rapid method for the determination of eight trichothecenes in chicken liver was developed based on a quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction an…
Determination of busulfan in human plasma using high-performance liquid chromatography with pre-column derivatization and fluorescence detection.
1999
A rapid, sensitive and reproducible high-performance liquid chromatographic assay for busulfan in human plasma was developed. After extraction of plasma samples with acetonitrile and methylene chloride, busulfan and the internal standard [1,5-bis(methanesulfonyloxy)pentane] were derivatized with 8-mercaptoquinoline to yield fluorescent compounds which were detected with a fluorescence detector equipped with filters of 360 nm (excitation) and 425 nm (emission). Calibration graphs showed a linear correlation (r>0.9990) over the concentration range of 20-2000 ng/ml. The recovery of busulfan from plasma standards was 70+/-5%. The detection and quantification limits for busulfan in plasma sample…
Comparison of liquid chromatography using triple quadrupole and quadrupole ion trap mass analyzers to determine pesticide residues in oranges.
2005
Liquid chromatography-triple quadrupole/mass spectrometry (LC-TQ/MS) and liquid chromatography-quadrupole ion trap/mass spectrometry (LC-QIT/MS) for determining bupirimate, hexaflumuron, tebufenpyrad, buprofezin, pyriproxyfen, and fluvalinate in fruits have been compared. The differences in the mass spectra obtained by triple and ion trap quadrupoles are discussed, showing how both of them provide interesting features. The evaluation of the two instruments was carried out by ethyl acetate extraction of oranges spiked with the studied pesticides at LOQ and 10 times the LOQ. Results obtained by LC-TQ/MS correlated well with those obtained by LC-QIT/MS. Recoveries were 70-94% by LC-TQ/MS and 7…
Calculation of chromatographic parameters by molecular topology: sulphamides
1994
This investigation was undertaken to test the ability of the molecular connectivity model to predict RF values in thin-layer chromatography (TLC) for a group of sulphamides using multi-variable regression equations with multiple correlation coefficients, standard error of estimate, F-Snedecor function values and Student's t-test as criteria of fit. Regression analyses showed that the molecular connectivity model predicts the values for this property in different silica gel stationary phases and different polar mobile phases. Corresponding stability and random studies were made on the selected prediction models which confirmed their goodness of fit. The results also demonstrated that differe…
Emerging approaches to estimate retention factors in high performance liquid chromatography.
2004
The retention factor is one of the most universally used parameters in chromatography. The errors associated with the conventional ways to determine the retention factor of compounds in liquid chromatography are studied and compared with those corresponding to new approaches. The later avoid the use of extra-column time and hold-up time values, which have proven to be tedious and ambiguous. Simulations and real data, used to examine the accuracy of four different approaches (two classic and two new), suggest that the new approaches could be considered more satisfactory than the classic ones.
Development of standard operation procedures for the manufacture of n-octadecyl bonded silicas as packing material in certified reference columns for…
2004
The development of standard operation procedures for the manufacture of a n-octadecyl bonded spherical silica packing from partially condensed tetraethoxysilane as silica source is described. The synthesis comprises five intermediate products and six synthesis steps which were examined according to their reproducibility and robustness. The results led to the optimisation of the manufacturing process for a n-octadecyl bonded silica. Correlations were drawn between the dynamic viscosity of the poly(ethoxy)siloxane (PES), the synthesis parameters, the resulting pore structural properties and particle size distribution of the silicas. Validated procedures were developed to manufacture spherical…
Multicommutation-NIR determination of Hexythiazox in pesticide formulations.
2006
A multicommutated flow-system was designed in order to increase analytical throughput and for controlling thermal effects on the NIR spectra for determination of Hexythiazox in pesticide formulations. An on-line standard addition was carried out showing the versatility and repeatability of multicommutation for the on-line mixing and dilution of solutions. Results obtained for commercial samples were statistically comparable with those obtained by an HPLC-reference method. Multicommutation-NIR allows the analysis of 52 samples per hour, in front of the 30 samples per hour analyzed by the NIR-batch procedure and the 7 samples per hour analyzed by HPLC-reference method.
New approaches based on modified Gaussian models for the prediction of chromatographic peaks
2012
Abstract The description of skewed chromatographic peaks has been discussed extensively and many functions have been proposed. Among these, the Polynomially Modified Gaussian (PMG) models interpret the deviations from ideality as a change in the standard deviation with time. This approach has shown a high accuracy in the fitting to tailing and fronting peaks. However, it has the drawback of the uncontrolled growth of the predicted signal outside the elution region, which departs from the experimental baseline. To solve this problem, the Parabolic-Lorentzian Modified Gaussian (PLMG) model was developed. This combines a parabola that describes the variance change in the peak region, and a Lor…
Prediction of peak shape as a function of retention in reversed-phase liquid chromatography
2004
Optimisation of the resolution of multicomponent samples in HPLC is usually carried out by changing the elution conditions and considering the variation in retention of the analytes, to which a standard peak shape is assigned. However, the change in peak shape with the composition of the mobile phase can ruin the optimisation process, yielding unexpected overlaps in the experimental chromatograms for the predicted optimum, especially for complex mixtures. The possibility of modelling peak shape, in addition to peak position, is therefore attractive. A simple modified-Gaussian model with a parabolic variance, which is a function of conventional experimental parameters: retention time (tR), p…