Determination of Formic Acid by Oxidation with Lead Tetraacetate

1954 ◽  
Vol 26 (6) ◽  
pp. 1053-1054 ◽  
Author(s):  
A. S. Perlin
Keyword(s):  
Formic Acid ◽  
Lead Tetraacetate

A CHEMICAL PROCEDURE FOR DETERMINATION OF THE C14-DISTRIBUTION IN LABELLED D-FRUCTOSE AND OTHER KETOSES

1957 ◽  
Vol 35 (1) ◽  
pp. 7-13 ◽  
Author(s):  
Carol Brice ◽  
A. S. Perlin
Keyword(s):  
Carbon Dioxide ◽  
Formic Acid ◽  
Glycolic Acid ◽  
Degradation Products ◽  
Lead Tetraacetate ◽  
The Individual ◽  
Chemical Procedure

A procedure is described for determining the activity of the individual carbon atoms in D-fructose labelled with C14, which is suitable for as little as 1 millimole of the sugar. The D-fructose is degraded by lead tetraacetate oxidation and the product is hydrolyzed to glycolic acid, formic acid, and D-glyceraldehyde. Glycolic acid is oxidized to formaldehyde (carbon-1) and carbon dioxide (carbon-2), and formic acid to carbon dioxide (carbon-3). D-Glyceraldehyde is degraded to carbon dioxide (carbons-4 and -5, combined) and formaldehyde (carbon-6); after reduction of a second portion of the D-glyceraldehyde to glycerol, the degradation products obtained are carbon dioxide (carbon-5) and formaldehyde (carbons-4 and -6, combined). The activity of carbon-1, -2, -3, -5, or -6 is thus determined directly, and of carbon-4 by difference in two ways. The procedure should also be applicable to C14-labelled L-sorbose. Lead tetraacetate oxidation of sedoheptulose followed by hydrolysis yields glycolic acid, formic acid, and D-erythrose. These three fragments are degraded in turn to afford a method for partial determination of the C14-distribution in samples of this important heptulose.

A CHEMICAL PROCEDURE FOR DETERMINATION OF THE C14-DISTRIBUTION IN LABELLED XYLOSE

1955 ◽  
Vol 33 (1) ◽  
pp. 368-373 ◽  
Author(s):  
Stewart A. Brown
Keyword(s):  
Carbon Dioxide ◽  
Formic Acid ◽  
Glycolic Acid ◽  
Periodic Acid ◽  
Glyoxylic Acid ◽  
Lead Tetraacetate ◽  
Carbon 14 ◽  
Chemical Procedure ◽  
Purified Salt

A series of reactions reported previously for the degradation of glucose has been modified and extended to permit the determination of carbon-14 in each of the five carbons of a single 2 mM. xylose sample. Methyl xylopyranoside was oxidized with periodic acid giving C-3 as formic acid, and a dialdehyde which was converted to strontium methoxy-diglycolate. The purified salt was hydrolyzed to glyoxylic and glycolic acids. The glyoxylic acid was isolated as the 2, 4-dinitrophenylhydrazone (C-1 + C-2) which was decarboxylated to give carbon dioxide from C-2. The glycolic acid was oxidized by lead tetraacetate to give C-4 as carbon dioxide and C-5 as formaldehyde. The activity in C-1 was determined by difference. The method was applied to xylose-1-C14, xylose-5-C14, and a biologically synthesized xylose sample with satisfactory results. This degradation procedure is theoretically applicable to other aldopentoses and aldotetroses.

A CHEMICAL PROCEDURE FOR DETERMINATION OF THE C14-DISTRIBUTION IN LABELLED D-FRUCTOSE AND OTHER KETOSES

1957 ◽  
Vol 35 (1) ◽  
pp. 7-13 ◽  
Author(s):  
Carol Brice ◽  
A. S. Perlin
Keyword(s):  
Carbon Dioxide ◽  
Formic Acid ◽  
Glycolic Acid ◽  
Degradation Products ◽  
Lead Tetraacetate ◽  
The Individual ◽  
Chemical Procedure

A procedure is described for determining the activity of the individual carbon atoms in D-fructose labelled with C14, which is suitable for as little as 1 millimole of the sugar. The D-fructose is degraded by lead tetraacetate oxidation and the product is hydrolyzed to glycolic acid, formic acid, and D-glyceraldehyde. Glycolic acid is oxidized to formaldehyde (carbon-1) and carbon dioxide (carbon-2), and formic acid to carbon dioxide (carbon-3). D-Glyceraldehyde is degraded to carbon dioxide (carbons-4 and -5, combined) and formaldehyde (carbon-6); after reduction of a second portion of the D-glyceraldehyde to glycerol, the degradation products obtained are carbon dioxide (carbon-5) and formaldehyde (carbons-4 and -6, combined). The activity of carbon-1, -2, -3, -5, or -6 is thus determined directly, and of carbon-4 by difference in two ways. The procedure should also be applicable to C14-labelled L-sorbose. Lead tetraacetate oxidation of sedoheptulose followed by hydrolysis yields glycolic acid, formic acid, and D-erythrose. These three fragments are degraded in turn to afford a method for partial determination of the C14-distribution in samples of this important heptulose.

A CHEMICAL PROCEDURE FOR DETERMINATION OF THE C14-DISTRIBUTION IN LABELLED XYLOSE

1955 ◽  
Vol 33 (3) ◽  
pp. 368-373 ◽  
Author(s):  
Stewart A. Brown
Keyword(s):  
Carbon Dioxide ◽  
Formic Acid ◽  
Glycolic Acid ◽  
Periodic Acid ◽  
Glyoxylic Acid ◽  
Lead Tetraacetate ◽  
Carbon 14 ◽  
Chemical Procedure ◽  
Purified Salt

A series of reactions reported previously for the degradation of glucose has been modified and extended to permit the determination of carbon-14 in each of the five carbons of a single 2 mM. xylose sample. Methyl xylopyranoside was oxidized with periodic acid giving C-3 as formic acid, and a dialdehyde which was converted to strontium methoxy-diglycolate. The purified salt was hydrolyzed to glyoxylic and glycolic acids. The glyoxylic acid was isolated as the 2, 4-dinitrophenylhydrazone (C-1 + C-2) which was decarboxylated to give carbon dioxide from C-2. The glycolic acid was oxidized by lead tetraacetate to give C-4 as carbon dioxide and C-5 as formaldehyde. The activity in C-1 was determined by difference. The method was applied to xylose-1-C14, xylose-5-C14, and a biologically synthesized xylose sample with satisfactory results. This degradation procedure is theoretically applicable to other aldopentoses and aldotetroses.

LC–MS/MS Determination of Apigenin in Rat Plasma and Application to Pharmacokinetic Study

2020 ◽  
Vol 21 ◽  
Author(s):  
Shixing Zhu ◽  
Jiayuan Zhang ◽  
Zhihua Lv ◽  
Mingming Yu
Keyword(s):  
Formic Acid ◽  
Pharmacokinetic Study ◽  
Ammonium Acetate ◽  
Rat Plasma ◽  
Biological Properties ◽  
Plasma Samples ◽  
Supply Rate ◽  
Natural Plant ◽  
Ammonium Acetate Buffer

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.

scholarly journals Determination of 19 Psychoactive Substances in Premortem and Postmortem Whole Blood Samples Using Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry

Separations ◽  
2021 ◽  
Vol 8 (6) ◽  
pp. 78
Author(s):  
Sevasti Karampela ◽  
Jessica Smith ◽  
Irene Panderi
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Formic Acid ◽  
Whole Blood ◽  
High Performance ◽  
Tandem Mass ◽  
Psychoactive Substances ◽  
Blood Samples ◽  
Whole Blood Samples

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.

Simultaneous Determination of Four Herbicide and Pesticide Residues in Chinese Green Tea Using QuEChERS Purification Procedure and UPLC-MS/MS Analysis

2013 ◽  
Vol 634-638 ◽  
pp. 1586-1590
Author(s):  
Su Fang Wang ◽  
Shou Jie Zhang ◽  
Chun Hong Dong ◽  
Guo Qing Wang ◽  
Jun Feng Guo ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Green Tea ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Graphitized Carbon Black ◽  
Ms Analysis ◽  
Relative Standard ◽  
Limit Of Quantitation

A method for simultaneous determination of residuals of four herbicides and pesticides, simazine, carboxin, diflubenzuron and rotenone, in Chinese green tea was developed. In the proposed method, the tea powder was placed in a centrifuge tube with a plug, extracted in saturated aqueous sodium chloride solution and acetonitrile, agitated using vortex oscillator, and then centrifuged 5 min at 4000 rpm. The supernatant solution was purified by primary secondary amine (PSA) sorbent, C18 power, and graphitized carbon black powder, respectively. Then the purified extracts were dissolved with acetonitrile:0.1% formic acid aqueous solution (40:60, V/V) and agitated, filtered using a syringe with 0.22 μm nylon filter prior to UPLC-MS/MS analysis. The UPLC analysis was performed on an ACQUITY UPLC® HSS T3 column (2.1 mm×100 mm, 1.8 µm), using acetonitrile-0.1% formic acid as mobile phase with the flow rate as 0.3 mL•min-1. Injection volume was 10 µL. Positive ionization mode was applied, and the ions were monitored in the multiple reaction monitoring (MRM) mode with curtain gas 0.069 MPa, collision gas 0.052 MPa, ESI ion spray voltage 5000 V, temperature 550 °C, nebulizer gas 0.24 MPa, and turbo gas 0.28 MPa. The limit of detection (LOD) and limit of quantitation (LOQ) of the proposed method are 1 μg•kg-1and 5 μg•kg-1, respectively. The average recoveries of the four pesticides at 10, 20, and 50 µg•kg-1spiking levels range from 77.4% to 95.3%. TheSupersSuperscript textcript textrelative standard deviation (RSD) (n=6) range form 11.83% to 4.52%.

A Headspace Gas Chromatographic Method for Determination of Formic acid Content in Isosulfan Blue and in Various Drugs

2021 ◽  
Vol 37 (2) ◽  
pp. 321-329
Author(s):  
Nilesh Takale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Rajarajan Govindasamy
Keyword(s):  
Sulfuric Acid ◽  
Formic Acid ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Class Iii ◽  
Drug Substances ◽  
Headspace Gas ◽  
Concentrated Sulfuric Acid ◽  
Gas Chromatographic Method

The Pharmaceutical industry uses formic acid in the manufacturing of various drug substances or API. At the time of manufacturing of API formic acid is use as an oxidizing agent. Formic acid is the simplest carboxylic acid. It also called methanoic acid.Formic acid present in API at high concentrations is very hazardous but in low concentrations is very beneficial. The developed and validated method was short, precise, cost effective and reproducible with FID detector and easy to use. The method is a selective and superficial analytical method for determination of formic acid in different drug substances. We report here the development and validation study of headspace gas chromatographic method to determine formic acid in different drug substances we are reported here. As per this method, the drug sample was dissolved in 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol (IPA) in a GC headspace vial and 0.1% (v/v) of concentrated sulfuric acid in isopropyl alcohol used as a diluent. A AB-Inowax capillary column (30 m x 0.32 mm I.D. and 0.5 µm film thickness) was used under gradient conditions with FID. The formic acid peak was well separated from all other solvents that are used in synthesis of particular drug substance. The LOD and LOQof the method for formic acid are 82 ppm and 249 ppm respectively. Formic acid are low toxic class-III solvent as per ICH guideline.

scholarly journals A HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY METHOD DEVELOPMENT FOR THE QUANTITATIVE DETERMINATION OF ENALAPRIL MALEATE FROM CACO-2 CELL MONOLAYERS

2018 ◽  
Vol 11 (7) ◽  
pp. 89
Author(s):  
Liliya Logoyda
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Formic Acid ◽  
High Performance ◽  
Liquid Chromatography Mass Spectrometry ◽  
Enalapril Maleate ◽  
Cell Monolayers ◽  
Chromatography Mass Spectrometry

Objective: A simple, rapid high-performance liquid chromatography-mass spectrometry (HPLC MS/MS) method was developed for the determination of enalapril maleate from confluent Caco-2 monolayers and aqueous solution.Methods: Chromatography was achieved on Discovery C18, 50×2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A [acetonitrile-water-formic acid, 5: 95:0.1 v/v] and eluent B [acetonitrile-formic acid, 100:0.1 v/v]). The initial content of the eluent B is 0%, which increases linearly by 1.0 min to 100% and 1.01 min returns to the initial 0%. The mobile phase was delivered at a flow rate of 0.4 ml/min into the mass spectrometer ESI chamber. The sample volume was 5 μl.Results: Under these conditions, enalapril maleate was eluted at 1.52 min. According to the Caco-2 test results, enalapril showed low permeability. It should be noted that the recovery value for enalapril is 100.62 %. Low in vitro permeability data for enalapril are in good agreement with the literature data.Conclusion: From results of the analysis, it can be concluded that developed method is simple and rapid for determination of enalapril maleate from confluent Caco-2 monolayers and aqueous solution. Acquired results demonstrate that proposed strategy can be effortlessly and advantageously applied for examination of enalapril from Caco-2 cell monolayers.

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