Development of a multi-sugar LC-MS/MS assay using simple chemical derivatization with acetic anhydride

2016 ◽  
Vol 8 (15) ◽  
pp. 3023-3033 ◽  
Author(s):  
Hermes Licea-Perez ◽  
Venkatraman Junnotula ◽  
Sylvia Zohrabian ◽  
Molly Karlinsey
Keyword(s):  
Acetic Anhydride ◽  
Chromatographic Separation ◽  
Chemical Derivatization ◽  
Carbohydrate Analysis ◽  
Simple Chemical

Carbohydrate analysis poses many analytical challenges, in terms of extraction, chromatographic separation, and detection.

scholarly journals Derivatizing Reagents for Detection of Organic Compounds By HPLC

2021 ◽  
pp. 1-13
Author(s):  
Pooja T. Chhanikar ◽  
Krishna R. Gupta ◽  
Milind J. Umekar
Keyword(s):  
Fluorescence Detection ◽  
Sulfonyl Chloride ◽  
Phenyl Isocyanate ◽  
Fluorescent Detection ◽  
Chemical Derivatization ◽  
Or Groups ◽  
Highly Sensitive ◽  
Simple Chemical ◽  
Derivatizing Agent ◽  
Uv Visible

Derivatization is the process of chemically modifying a compound to develope a new compound which has properties that are suitable for analysis using HPLC. Derivatization improves the detectability of a target analyte by reaction with suitable derivatizing agent. Derivatization reactions are simple chemical modification of substance that make it compatible with the selected separation method or transforms substance with a low UV- absorption into highly sensitive product. Derivatization reactions in liquid chromatography modify the solutes adding a chomophore for easy UV detection or a fluorophore for sensitive fluorescent detection. The chemical structure of the compound remains same and just modifies the specific functional group for reacting compounds to derivative of deviating chemical and physical properties in order to make them detectable. Introduction of certain elements or groups through chemical derivatization may enhance the detector’s response helpful for the elucidation of structure of analytes. In conclusion, the present review describe various derivatization reagents for pre-column and post column derivatization process in HPLC by UV-visible and fluorescence detection are summarized along with reactions and some practical aspects. The commonly used derivatizing reagents in HPLC are 1-fluoro-2, 4-dinitrobenzene, ninhydrine, 4-N-N-dimethylaminoazobenzene-4’-sulfonyl chloride, benzoyl chloride, phenyl isocyanate for UV-visible detection and o-phthalaldehyde, fluorescamine, 1-dimethylaminonapthalene-5-sulfonyl chloride (DNS-Cl), 9-fluorenylmethyl chloroformate (Fmoc-Cl), benzofurans for Fluorescence detection.

The Acetic Anhydride-Sulphuric Reaction for General Paresis

1927 ◽  
Vol 73 (302) ◽  
pp. 419-421 ◽  
Author(s):  
A. G. Duncan
Keyword(s):  
Acetic Anhydride ◽  
Mental Disorder ◽  
Sulphuric Acid ◽  
Positive Reaction ◽  
Chemical Reaction ◽  
Spinal Fluid ◽  
General Paresis ◽  
Simple Chemical

While elaborating a test for cholesterol in the cerebro-spinal fluid, 0. H. Boltz (I) observed and investigated a reaction which occurred predominantly in cases of neuro-syphilis, and which he named the acetic anhydride-sulphuric test. To I c.c. of spinal fluid was added 03 c.c. of acetic anhydride, drop by drop, and after mixing the fluids by shaking, [email protected]. of concentrated sulphuric acid was added in drops, and the mixture shaken again. The development of a blue pink or lilac colour characterized a positive reaction. The test has been studied in this country, and it has been claimed that the reaction is positive in almost every case of general paresis, and negative in almost every other type of mental disorder, except certain cases of non-paretic neuro-syphilis. As this constitutes a surprising degree of specificity of an apparently simple chemical reaction for a single disease, I have carried out the reaction in association with the routine tests in a series of cerebro-spinal fluids with a view to ascertaining its value. One hundred and sixty fluids were examined—a comparatively small number on which to base conclusions, but the results will show that the claims previously advanced for the value of the test require considerable modification.

Epimerization of Monosaccharides in Acetic Acid and Acetic Anhydride. Synthesis of D-Altrose

1972 ◽  
Vol 50 (7) ◽  
pp. 1092-1094 ◽  
Author(s):  
Walter Sowa
Keyword(s):  
Acetic Acid ◽  
Sulfuric Acid ◽  
Acetic Anhydride ◽  
Chromatographic Separation ◽  
Reaction Conditions

Acetolysis of 1,2;5,6-di-O-isopropylidene-α-D-allofuranose occurred with inversion at C-2 in a medium composed of acetic acid, acetic anhydride, and sulfuric acid. D-Altrose was isolated in 45% yield by deacetylation and chromatographic separation of the mixture of products. Unsubstituted D-allose did not epimerize under the same reaction conditions.

Selective mass spectrometric analysis of thiols using charge-tagged disulfides

The Analyst ◽  
2016 ◽  
Vol 141 (19) ◽  
pp. 5520-5526 ◽  
Author(s):  
Eric Janusson ◽  
G. Bryce McGarvey ◽  
Farhana Islam ◽  
Christine Rowan ◽  
J. Scott McIndoe
Keyword(s):  
Mass Spectrometry ◽  
Electrospray Ionization ◽  
Electrospray Ionization Mass Spectrometry ◽  
Mass Spectrometric ◽  
Mass Spectrometric Analysis ◽  
Spectrometric Analysis ◽  
Ionization Mass ◽  
Chemical Derivatization ◽  
Complex Matrix ◽  
Simple Chemical

A simple chemical derivatization technique was developed for electrospray ionization mass spectrometry (ESI-MS) in which thiols and disulfides may be selectively analyzed in a complex matrix and easily characterized.

Chemical Derivatization Analysis of Pesticide Residues. VIII. Analysis of 15 Chlorophenols in Natural Water by In Situ Acetylation

1984 ◽  
Vol 67 (4) ◽  
pp. 789-794
Author(s):  
Hing-Biu Lee ◽  
Li-Da Weng ◽  
Alfred S Y Chau
Keyword(s):  
Gas Chromatography ◽  
Quantitative Analysis ◽  
Acetic Anhydride ◽  
Petroleum Ether ◽  
Natural Water ◽  
Analytical Method ◽  
Pesticide Residues ◽  
Natural Waters ◽  
Chemical Derivatization

Abstract A rapid analytical method is presented for quantitative analysis of 15 chlorophenols in natural waters by in situ acetylation. In the presence of KHC03, phenols in water are acetylated by acetic anhydride directly without pre-extraction. The resultant acetates are extracted by petroleum ether and analyzed by electron capture gas chromatography. The investigation to optimize the conditions for in situ acetylation of these phenols is also described. This method has been validated and shown to be applicable over a range from 100 to 0.01 ppb with a 1 L water sample.

scholarly journals LC–HRMS and Chemical Derivatization Strategies for the Structure Elucidation of Caribbean Ciguatoxins: Identification of C-CTX-3 and -4

Marine Drugs ◽  
2020 ◽  
Vol 18 (4) ◽  
pp. 182 ◽  
Author(s):  
Fedor Kryuchkov ◽  
Alison Robertson ◽  
Christopher O. Miles ◽  
Elizabeth M. Mudge ◽  
Silvio Uhlig
Keyword(s):  
Chemical Characterization ◽  
Diagnostic Value ◽  
Chemical Derivatization ◽  
Oxidation Reactions ◽  
Structural Modifications ◽  
Low Concentrations ◽  
Simple Chemical ◽  
Product Ions ◽  
Mass Spectrometric Fragmentation

Ciguatera poisoning is linked to the ingestion of seafood that is contaminated with ciguatoxins (CTXs). The structural variability of these polyether toxins in nature remains poorly understood due to the low concentrations present even in highly toxic fish, which makes isolation and chemical characterization difficult. We studied the mass spectrometric fragmentation of Caribbean CTXs, i.e., the epimers C-CTX-1 and -2 (1 and 2), using a sensitive UHPLC–HRMS/MS approach in order to identify product ions of diagnostic value. We found that the fragmentation of the ladder-frame backbone follows a characteristic pattern and propose a generalized nomenclature for the ions formed. These data were applied to the structural characterization of a pair of so far poorly characterized isomers, C-CTX-3 and -4 (3 and 4), which we found to be reduced at C-56 relative to 1 and 2. Furthermore, we tested and applied reduction and oxidation reactions, monitored by LC–HRMS, in order to confirm the structures of 3 and 4. Reduction of 1 and 2 with NaBH4 afforded 3 and 4, thereby unambiguously confirming the identities of 3 and 4. In summary, this work provides a foundation for mass spectrometry-based characterization of new C-CTXs, including a suite of simple chemical reactions to assist the examination of structural modifications.

DETERMINATION OF MICRO-AMOUNTS OF 5β-PREGNAN-3α-OL-20-ONE IN URINE USING INFRARED-SPECTROMETRY

1962 ◽  
Vol 41 (2) ◽  
pp. 234-246 ◽  
Author(s):  
H. J. van der Molen
Keyword(s):  
Infrared Spectrum ◽  
Quantitative Determination ◽  
Acid Hydrolysis ◽  
Chromatographic Separation ◽  
Pure Form ◽  
Infrared Spectrometry ◽  
Hydrolysis Of

ABSTRACT A procedure for the quantitative determination of 5β-pregnan-3α-ol-20-one in urine is described. After acid hydrolysis of the pregnanolone-conjugates in urine, the free steroids are extracted with toluene. Pregnanolone is isolated in a pure form as its acetate; after chromatographic separation of the free steroids on alumina, the fraction containing pregnanolone is acetylated and rechromatographed on alumina. Quantitative determination of the isolated pregnanolone-acetate is carried out with the aid of the infrared spectrum recorded by a micro KBr-wafermethod. The reliability of the method under various conditions is discussed under the headings, specificity, accuracy, precision and sensitivity. It is possible to determine 30–40 μg pregnanolone in a 24-hours urine portion with a precision of 25%.

Sign in / Sign up

Export Citation Format

Share Document