Abstract
We have developed a sensitive, simple and cheap method for determination of lipoic acid in urine and dietary supplement tablets. The method is based on conversion of lipoic acid to its thiol counterpart – dihydrolipoic acid – by reductive cleavage with tris(2-carboxyethyl)phosphine hydrochloride prior to precolumn derivatization with 1-benzyl-2- chloropyridinium bromide, followed by ion-pairing reversed-phase liquid chromatography separation and ultraviolet detection of its 2-S-pyridinium derivative at 321 nm. Bathochromic shift from the reagent absorption maximum at 275 nm to that of derivative maximum at 321 nm, taking place during reaction, is analytically advantageous. In developing this method the following parameters were investigated and optimized: the time, pH and reagent excess in the derivatization step and mobile phase buffer concentration, pH, organic modifier and column temperature in the separation step. Calibration plot, understood as the relationship between instrument response and known concentration of the analyte, demonstrated linearity of results when applied to normal urine spiked with growing amounts of lipoic acid within the tested range 0.2 – 50 µmol/L. The method was validated for urine samples received from healthy donors and urine concentration of lipoic acid was monitored after oral administration of 600 mg of lipoic acid.
Keywords: Derivatization, determination, disulfide, HPLC, lipoic acid, thiol, urine.
Current Analytical Chemistry
Title:Determination of Lipoic Acid in the form of 2-S-pyridinium Derivative by High-performance Liquid Chromatography with Ultraviolet Detection
Volume: 10 Issue: 3
Author(s): Grazyna Chwatko, Pawel Kubalczyk and Edward Bald
Affiliation:
Keywords: Derivatization, determination, disulfide, HPLC, lipoic acid, thiol, urine.
Abstract: We have developed a sensitive, simple and cheap method for determination of lipoic acid in urine and dietary supplement tablets. The method is based on conversion of lipoic acid to its thiol counterpart – dihydrolipoic acid – by reductive cleavage with tris(2-carboxyethyl)phosphine hydrochloride prior to precolumn derivatization with 1-benzyl-2- chloropyridinium bromide, followed by ion-pairing reversed-phase liquid chromatography separation and ultraviolet detection of its 2-S-pyridinium derivative at 321 nm. Bathochromic shift from the reagent absorption maximum at 275 nm to that of derivative maximum at 321 nm, taking place during reaction, is analytically advantageous. In developing this method the following parameters were investigated and optimized: the time, pH and reagent excess in the derivatization step and mobile phase buffer concentration, pH, organic modifier and column temperature in the separation step. Calibration plot, understood as the relationship between instrument response and known concentration of the analyte, demonstrated linearity of results when applied to normal urine spiked with growing amounts of lipoic acid within the tested range 0.2 – 50 µmol/L. The method was validated for urine samples received from healthy donors and urine concentration of lipoic acid was monitored after oral administration of 600 mg of lipoic acid.
Export Options
About this article
Cite this article as:
Chwatko Grazyna, Kubalczyk Pawel and Bald Edward, Determination of Lipoic Acid in the form of 2-S-pyridinium Derivative by High-performance Liquid Chromatography with Ultraviolet Detection, Current Analytical Chemistry 2014; 10 (3) . https://dx.doi.org/10.2174/1573411010999131219101340
DOI https://dx.doi.org/10.2174/1573411010999131219101340 |
Print ISSN 1573-4110 |
Publisher Name Bentham Science Publisher |
Online ISSN 1875-6727 |
Call for Papers in Thematic Issues
Advancements in biomedicine, corrosion inhibition/monitoring, and lubrication of carbon dots
Carbon dots, a class of carbon-based nanomaterials, have garnered substantial interest in various scientific and engineering fields due to their unique properties, including excellent optical properties, outstanding biocompatibility, easy preparation, good dispersity, ultrasmall size, low toxicity and environmental friendliness. This special issue of Current Analytical Chemistry aims to showcase cutting-edge ...read more
Analytical methods for environmental and food analysis
In recent years, the study of the chemical composition of food and the environment depends on analytical methods in order to acquire information about the chemical composition, processing, quality control and contamination of soil, water, air, plants and foods, aspects very important for food safety and environmental quality control. There ...read more
Applications of artificial intelligence in chemical analysis
Artificial intelligence (AI) has demonstrated its versatility in almost all scientific fields, especially analytical chemistry, which is leading the way in the integration of AI. According to Chemical Abstract Services, one of the major disciplines contributing to AI-related publications and patents is analytical chemistry. That?s because techniques such as deep ...read more
Bioanalytical and Biosensor Technologies for Target Molecules
Bioanalytical and biosensor technologies constitute the core of detecting and sensing diverse molecules within living organisms, encompassing proteins, DNA, small molecular metabolites, and beyond. These molecules assume pivotal roles in biological processes, rendering their analysis and sensing indispensable for comprehending biological phenomena and unraveling disease mechanisms. In the current landscape ...read more
- Author Guidelines
- Graphical Abstracts
- Fabricating and Stating False Information
- Research Misconduct
- Post Publication Discussions and Corrections
- Publishing Ethics and Rectitude
- Increase Visibility of Your Article
- Archiving Policies
- Peer Review Workflow
- Order Your Article Before Print
- Promote Your Article
- Manuscript Transfer Facility
- Editorial Policies
- Allegations from Whistleblowers
Related Articles
-
Calcium Ion – The Key Player in Cerebral Ischemia
Current Medicinal Chemistry Cellular and Functional Effects of Insulin Based Therapies and Exercise on Endothelium
Current Pharmaceutical Design Clinical Uses of 1-Alpha-Hydroxy-Ergocalciferol
Current Vascular Pharmacology Development of Nitric Oxide Donors for the Treatment of Cardiovascular Diseases
Cardiovascular & Hematological Agents in Medicinal Chemistry Prophylactic Neuroprotection
Current Drug Targets Development of Nanocomponent Ointment Composition for the Treatment of Various Etiologies Wounds
Current Nanomedicine Hyperuricemia and Hypertension — A Causal Relationship Ignored For All Too Long
Current Hypertension Reviews Antidiabetic Potential of Fabaceae Family: An Overview
Current Nutrition & Food Science The Malignant Obesity Hypoventilation Syndrome (MOHS)
Current Respiratory Medicine Reviews Structure, Function and Biological Relevance of Prolyl Oligopeptidase
Current Protein & Peptide Science MicroRNAs in Cardiovascular Therapeutics
Current Topics in Medicinal Chemistry Marine Peptides and Related Compounds in Clinical Trial+
Anti-Cancer Agents in Medicinal Chemistry Expression and Function of Cytokines and Chemokines in Neuropsychiatric Related Systemic Lupus Erythematosus
Current Rheumatology Reviews Nutriproteomics – Linking Proteomics Variation with Personalized Nutrition
Current Pharmacogenomics and Personalized Medicine Editorial [Hot Topic: Recent Advances and Future Prospect in Protease Targeting (Executive Editor: B. Turk) ]
Current Pharmaceutical Design The Effect of Antihypertensive Drugs on Carotid Intima Media Thickness: An Up-to-Date Review
Current Medicinal Chemistry The Angiotensin Converting Enzyme 2 (ACE2), Gut Microbiota, and Cardiovascular Health
Protein & Peptide Letters Metabolic Syndrome: Sex-Related Cardiovascular Risk and Therapeutic Approach
Current Medicinal Chemistry Optimizing the Management of Uncontrolled/Resistant Hypertension. The Importance of Sleep Apnoea Syndrome
Current Vascular Pharmacology Anticoagulation in Patients with Heart Failure
Cardiovascular & Hematological Agents in Medicinal Chemistry