scholarly journals Determination of citric and oxalic acid in fungi fermentation broth through HPLC-DAD and solid-phase extraction

DYNA ◽  
2020 ◽  
Vol 87 (212) ◽  
pp. 26-30
Author(s):  
Laura Marcela Trujillo Vargas ◽  
Yesid Hernan Vélez Salazar ◽  
Margarita Enid Ramírez Carmona
Keyword(s):  
Oxalic Acid ◽  
Organic Acids ◽  
Solid Phase ◽  
Fermentation Broth ◽  
Preparation Technique ◽  
Liquid Chromatograph ◽  
Ion Exclusion ◽  
Validation Parameters ◽  
Fermentation Broths

This work describes a method for the simultaneous determination of organic acids in fungi fermentation broths. The sample preparation technique and the chromatographic conditions were optimized to enable the monitoring of the fermentation process. The determination of the citric and oxalic acid was done with a high resolution liquid chromatograph adapted to a detector with diode arrangement, an IC-Pak Ion-Exclusion 7μm (7.8 x 300 mm) column and a mobile phase of 0.001N H2SO4 with isocratic elusion. The validation parameters show efficiency, adequate linearity, and standard deviation values (%RSD) from 0.018% and 4.650%. the quantification limits (LDC) were 50.76 mg/L for citric acid and 20.18 mg/L for oxalic acid and the detection limits (LDD) were 0.6 mg/L for both acids. The method was applied in the analysis of organic acids in fermentation broths of Aspergillus niger.

scholarly journals Oxytetracycline Residues in Honey Analyzed by Liquid Chromatography with UV Detection

2013 ◽  
Vol 57 (1) ◽  
pp. 25-32 ◽  
Author(s):  
Anna Gajda ◽  
Andrzej Posyniak ◽  
Andrzej Bober ◽  
Tomasz Błądek ◽  
Jan Żmudzki
Keyword(s):  
Liquid Chromatography ◽  
Oxalic Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Experimental Treatment ◽  
Uv Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method

Summary A liquid chromatography method with UV detection for determination of oxytetracycline (OTC) in honey has been developed. The samples were extracted with the solution of oxalic acid. The clean-up procedure was performed by solid phase extraction (SPE) using polymeric Strata X and carboxylic acid cartridges. Chromatographic separation was carried out on the Luna C8 analytical column with mobile phase consisting of acetonitrile-0.02 M oxalic acid. The method has been successfully validated according to the requirements of the European Decision 2002/657/EC and this method is used in routine control of oxytetracycline in honey samples. The limit of detection (LOD) and limit of quantification (LOQ) of the presented method were 10 and 12.5 μg/kg, respectively. The developed method has also been verified in quantitative determination of oxytetracycline residues in honey after experimental treatment with this product in bee colonies.

scholarly journals Multiresidue Method for N-Methyl Carbamates and Metabolite Pesticide Residues at the Parts-per-Billion Level in Selected Representative Commodities of Fruit and Vegetable Crop Groups

2004 ◽  
Vol 87 (5) ◽  
pp. 1237-1251 ◽  
Author(s):  
Lynda V Podhorniak ◽  
Frank J Schenck ◽  
Alexander Krynitsky ◽  
Francis Griffith ◽  
Francis Griffith
Keyword(s):  
Environmental Protection Agency ◽  
Solid Phase ◽  
Reversed Phase ◽  
Mass Spectrometric ◽  
Fruit And Vegetable ◽  
Vegetable Crop ◽  
Additional Material ◽  
Liquid Chromatograph ◽  
Mass Spectrometric Detector

Abstract A reversed-phase liquid chromatographic method with both fluorescence and mass spectrometric detection is presented for the determination of 13 parent N-methyl carbamate pesticides and their metabolites, as well as piperonyl butoxide, for a total of 24 compounds in selected fruits and vegetables. The commodities chosen were of special concern to the U.S. Environmental Protection Agency (EPA) because they had the least amount of monitoring data for dietary exposure estimates used in risk assessment. The method is based on a judicious selection of procedures from U.S. Food and Drug Administration sources such as the Pesticide Analytical Manual (Volume I), and Laboratory Information Bulletins, plus additional material from the chemical literature combined in a manner to recover the N-methyl carbamates and their metabolites at the 1 μg/kg or 1 part-per-billion level. The method uses an acetone extraction, followed by an aminopropyl solid-phase extraction cleanup. Determination of residues is by RP-LC, in which the liquid chromatograph is interfaced with either a fluorescence or a mass spectrometric detector. The method is designed so that a set of 6 samples can be prepared in 1 working day for overnight instrumental analysis. Recovery data are presented from analyses of selected commodities in some of EPA's fruit and vegetable crop groupings. A table listing relative retention times is presented for the N-methyl carbamates and their metabolites.

scholarly journals Extending Metabolomic Studies of Apis mellifera Venom: LC-MS-Based Targeted Analysis of Organic Acids

Toxins ◽  
2019 ◽  
Vol 12 (1) ◽  
pp. 14
Author(s):  
Magdalena Pawlak ◽  
Agnieszka Klupczynska ◽  
Zenon J Kokot ◽  
Jan Matysiak
Keyword(s):  
Citric Acid ◽  
Organic Acids ◽  
Kynurenic Acid ◽  
Glutaric Acid ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Dry Weight ◽  
Triple Quadrupole Mass Spectrometer ◽  
Targeted Analysis

Organic acids are important active small molecules present in venoms and toxins, which have not been fully explored yet. The aim of the study was the determination of organic acids in honeybee venom (HBV) samples by using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Two protocols for sample preparation were employed. A solid-phase extraction was used for the determination of malonic acid, fumaric acid, glutaric acid, and kynurenic acid. A dilute-and-shoot method was optimal for: citric acid, malic acid, and succinic acid. Chromatographic separation was performed using a Synergi Hydro-RP column. Detection was performed on a triple-quadrupole mass spectrometer operating in multiple reaction monitoring mode. Among the analytes, glutaric acid and kynurenic acid were present in HBV samples in the lowest concentrations, whereas citric acid was the most abundant acid in each sample, and accounted for an average of 86 mg/g (8.6%) of the venom dry weight. Organic acids were discussed in terms of function. This is the first study in the available literature that provides specific data on the content of organic acids in HBV using a validated quantitative method.

scholarly journals Rapid MSPD-LC–MS/MS Procedure for Determination of Pesticides in Potato Tubers

2020 ◽  
Vol 58 (9) ◽  
pp. 831-843
Author(s):  
Magdalena Danek ◽  
Marcin Sajdak ◽  
Joanna Płonka ◽  
Hanna Barchańska
Keyword(s):  
Analytical Procedure ◽  
Solid Phase ◽  
Potato Tubers ◽  
Limit Of Quantification ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
Validation Parameters ◽  
Dispersion Technique

Abstract The program of potato protection recommended by the producers of agrochemicals requires application: thiamethoxam, lambda-cyhalothrin, deltamethrin, rimsulfuron and metalaxyl. Therefore, there is a risk that these pesticides are present in tubers, thus posing a toxicological risk to the consumer. In this respect, it is necessary to monitor the presence of these compounds in edible plants. Therefore, the aim of this paper was to develop a novel, simple and robust analytical procedure for simultaneous determination of above-mentioned pesticides in potato tubers. To develop an analytical procedure that fulfills SANTE demands, quick, easy, cheap, effective, rugged and safe method and matrix solid phase dispersion technique were investigated. The final determination was conducted by liquid chromatography with tandem mass spectrometry. The obtained experimental data were analyzed by analysis of variance. For the extraction of analytes, matrix solid phase dispersion with octadecyl sorbent and methanol as eluent was chosen, since it provides the validation parameters according to SANTE requirements (recovery: 77–111%, relative standard deviation: 1–10%, limit of quantification: 0.9–5.0 μg/kg). This innovative analytical procedure is a practical analytical tool, which was successfully proven by applying it for target pesticides determination in potato tuber samples of different varieties randomly chosen at local markets.

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