Spectrophotomhtric Determination of Vanadium with Salicylic Acid in Formic Acid Medium

1985 ◽  
Vol 18 (14) ◽  
pp. 1733-1742
Author(s):  
Anna C. P. Baptista ◽  
Henrique A. Salles andrade
Author(s):  
Shixing Zhu ◽  
Jiayuan Zhang ◽  
Zhihua Lv ◽  
Mingming Yu

Background: Apigenin, a natural plant flavone, has been shown to possess a variety of biological properties. Objective: In this report, a highly selective and sensitive LC-MS/MS method was developed and validated for the determination of apigenin in rat plasma. Methods: Analysts were separated on the HSS T3 column (1.8 μm 2.1×100 mm) using acetonitrile and 0.1% formic acid in 2 mM ammonium acetate buffer at a supply rate of 0.200 mL/min as eluent in gradient model. Results: Plasma samples were treated by protein precipitation using acetonitrile for the recovery ranging from 86.5% to 90.1% for apigenin. The calibration curves followed linearity in the concentration range of 0.50-500 ng/mL. The inter-day and intra-day precisions at different QC levels within 13.1% and the accuracies ranged from -10.6% to 8.6%. Conclusion: The assay has been successfully applied to the pharmacokinetic study of apigenin in rats.


Separations ◽  
2021 ◽  
Vol 8 (6) ◽  
pp. 78
Author(s):  
Sevasti Karampela ◽  
Jessica Smith ◽  
Irene Panderi

An ever-increasing need exists within the forensic laboratories to develop analytical processes for the qualitative and quantitative determination of a broad spectrum of new psychoactive substances. Phenylethylamine derivatives are among the major classes of psychoactive substances available on the global market and include both amphetamine analogues and synthetic cathinones. In this work, an ultra-high-performance liquid chromatography-positive ion electrospray ionization tandem mass spectrometric method (UHPLC-ESI-MS/MS) has been developed and fully validated for the determination of 19 psychoactive substances, including nine amphetamine-type stimulants and 10 synthetic cathinone derivatives, in premortem and postmortem whole blood. The assay was based on the use of 1 mL premortem or postmortem whole blood, following solid phase extraction prior to the analysis. The separation was achieved on a Poroshell 120 EC-C18 analytical column with a gradient mobile phase of 0.1% formic acid in acetonitrile and 0.1% formic acid in water in 9 min. The dynamic multiple reaction monitoring used in this work allowed for limit of detection (LOD) and lower limit of quantitation (LOQ) values of 0.5 and 2 ng mL−1, respectively, for all analytes both in premortem and postmortem whole blood samples. A quadratic calibration model was used for the 12 quantitative analytes over the concentration range of 20–2000 ng mL−1, and the method was shown to be precise and accurate both in premortem and postmortem whole blood. The method was applied to the analysis of real cases and proved to be a valuable tool in forensic and clinical toxicology.


1976 ◽  
Vol 59 (4) ◽  
pp. 807-810
Author(s):  
Jeffrey C Hamm

Abstract The USP analysis for procainamide HCl is titrimetric and relatively nonspecific, capsule and tablet dyes may interfere, and the method is not applicable to coated tablets. In the spectrophotofluorometric method the sample deteriorates when exposed to a xenon source. In the ultraviolet spectrophotometric method reported here, the sample is dispersed in acid medium, possible interferences are extracted in chloroform, base is added, procainamide is extracted in chloroform, the residue is dissolved in sodium hydroxide, and the compound is measured by absorption at 272 nm and comparison with a standard. Recoveries of standards added to capsule, tablet, and injection composites ranged from 99.3 to 102%. Twelve collaborators reported duplicate assay results for all 3 dosage forms with per cent standard deviations for 5 samples ranging from 1.01 to 1.27%. The method has been adopted as official first action.


Soil Research ◽  
1989 ◽  
Vol 27 (4) ◽  
pp. 663 ◽  
Author(s):  
EA Close ◽  
HKJ Powell

This paper examines the use of short extraction times, and the determination of aluminium with chrome azurol S (CAS), for the estimation of 0.02 M CaCl2-soluble aluminium in soils. It reports the correlation between CAS-reactive aluminium in 5 min extracts and percent maximum yield of white clover (Trifolium repens) for a series of acid soils. The reactivity of soluble and colloidal aluminium species with the metallochromic reagent CAS has been assessed. ~ l ( a q ) ~ + , simple hydroxy species and complexes of weakly binding ligands (salicylic acid, tannins) are CAS-reactive (2 rnin). In contrast, complexes of strongly binding ligands (citric acid, fulvic acid) are not CAS-reactive ([Al] ~ [L] ~ [CAS] ~ 1-2~10-5 M). For a series of six limed phosphated topsoils and subsoils (pH 4.2-5.5), 0.02 M CaCl2- soluble aluminium, as determined with CAS, was negatively correlated against the percent maximum yield of white clover; r2 = -0.73** (5 min extraction), n = 20. This correlation is similar to that for yield against total aluminium as determined by atomic absorption spectroscopy after 60 min extraction (r2 = -0.77**). However, the colorimetric analysis is more convenient and sensitive; further, it does not measure colloidal and polymeric aluminium species (which may not be plant-available). The satisfactory correlation achieved for short extraction times suggests use of CAS for a rapid field method for aluminium toxicity in soils.


The Analyst ◽  
1976 ◽  
Vol 101 (1208) ◽  
pp. 867
Author(s):  
J. P. Sharma ◽  
V. K. S. Shukla ◽  
A. K. Dubey

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