Search results for "Standard addition"
showing 10 items of 72 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…
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…
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.
Determination of theophylline and paraxanthine in urine samples by liquid chromatography using the H-point standard additions method
1992
Abstract The simultaneous determination of theophylline and paraxanthine in urine samples by the H-point standard additions method (HPSAM) is described. Samples are extracted with C 18 solid-phase extraction cartridges and chromatographed using a Hypersil C 18 -ODS column and a mobile phase consisting of acetonirile-phosphate buffer in the gradient elution mode. Under these conditions theophylline and paraxanthine are eluted with short retention times. Although their chromatographic peaks are overlapped and their spectra are very similar, the H-point standard additions method provides excellent results in the determination of both xanthines at therapeutic levels.
Free fatty acids and other volatile compounds for the characterisation of “Vastedda della valle del Belìce” cheese Acidos grasos libres y otros const…
2010
The analysis of the volatile constituents of “Vastedda della valle del Belice”, a typical Sicilian pasta filata cheese, was performed using solid phase microextraction and high-resolution gas chromatography/mass spectrometry. The research aimed to verify if the volatile fraction, determinant for cheese flavor, differs among producers and/or production seasons. The samples were provided by four producers from the area of the Protected Designation of Origin (PDO) production, during two different seasons of production. A total of 42 volatile components were identified: the main components were found to be butanoic, hexanoic, octanoic, and decanoic acid. Free fatty acids were quantified using t…
H-point standard additions method for resolution of overlapped chromatographic peaks with a conventional fluorescence detector. Determination of phen…
1996
The H-Point Standard Additions Method (HPSAM) is proposed in order to resolve overlapping peaks in liquid chromatography by using a conventional fluorescence detector. The method uses as analytical signals the heights or the areas obtained at two previously selected emission wavelengths, and good results are obtained for highly overlapping peaks with highly overlapping fluorescence spectra. The principal benefits of the method are the ease of finding the required wavelengths, its insensitivity to changes in the retention time of the peak from one injection to another, and the possibility of using it in highly or only partially overlapping peaks. We have applied the method to the determinati…
Comparative Study on the Determination of Cephalexin in its Dosage Forms by Spectrophotometry and HPLC with UV-vis Detection
1997
This paper discusses the spectrophotometric determination of cephalexin as the intact cephalexin or as its acid-induced degradation product. Cephalexin can be determined in the range 1 × 10−5−18 × 10−5M with relative standard deviations of 5-1%. The limits of quantitation and detection were 10−5 and 0.3 × 10−5M, respectively. These procedures were compared with reversed-phase HPLC determination. No interference was observed in the presence of common pharmaceutical adjuvants. The H-point standard additions method was applied in order to correct for the possible presence of the cephalexin precursor, 7-aminocephalosporanic acid; this improves the selectivity of the UV-vis spectrophotometric me…
A comparison of various calibration techniques applied to the ninhydrin-cefoxitin determination
1996
Abstract This report deals with spectrophotometric determination of cefoxitin from intact antibiotics or from its acid induced degradation product by means of their reaction with ninhydrin in a strong sulphuric acid medium. To obtain the calibration graphs four methods were used: absorbance of reacted cefoxitin against a reagent blank as an analytical signal, first-derivative signal of absorbance against a water blank as an analytical signal, first-derivative signal of absorbance against a reagent blank as an analytical signal and the H-Point Standard Additions Method (HPSAM) by using absorbance increment values as analytical signals. The HPSAM is applied to the determination of cefoxitin i…
Development of the H-point standard additions method for coupled liquid chromatography and UV-visible spectrophotometry
1992
Abstract This work establishes the fundamentals of the H-point standard additions method for liquid chromatography for the simultaneous analysis of binary mixtures with overlapped chromatographic peaks. The method was compared with the deconvolution method of peak suppression and the second derivative of elution profiles. Different mixtures of diuretics were satisfactorily resolved.
Determination of chromium in treated crayfish,Procambarus clarkii, by Electrothermal AAS: Study of chromium accumulation in different tissues
1986
In the present study, the authors investigated the accumulation of chromium in muscle, hepatopancreas, antennal glands, and gills of Procambarus clarkii (Girard) from Lake Albufera following Cr(VI)-exposure. Determinations of chromium were made by using Electrothermal Atomic Absorption Spectroscopy and the standard additions method.