What is Mstfa used for?
N-Methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) is a very versatile reagent because it can be used to derivatize many of the functional groups commonly found in organic compounds. It operates by attachment of a nonpolar trimethylsilyl (TMS) group (Figure 1).
What is a silylation reaction?
Silylation is the introduction of a (usually) substituted silyl group (R3Si) to a molecule. The process is the basis of organosilicon chemistry.
What is Bstfa?
BSTFA (N,O-bis(trimethylsilyl)trifluoroacetamide) is the pre- ferred reagent for trimethylsilylation of alcohols, alkaloids, amines and biogenic amines, carboxylic acids, phenols, and steroids.
Why is it important to do the derivatization before performing a GC analysis?
The derivatization is typically done to change the analyte properties for a better separation and also for enhancing the method sensitivity. In GC/MS, derivatization may improve the capability of compound identification.
What is derivatization in GC analysis?
Derivatization is the process of chemically altering an analyte or analytes. Laboratorians often choose to derivatize particular analytes in order to improve their chromatography, thermal stability, or their identification. Derivatization for GC-MS typically involves silylation, alkylation, or acylation reactions.
What is a silylating agent?
Silylating agents are silicon-based chemicals that are used to modify organic and inorganic substrates to impart physical and chemical modifications to those substrates.
What is a derivatizing agent?
Derivatization is a technique used in chemistry which converts a chemical compound into a product (the reaction’s derivate) of similar chemical structure, called a derivative. Resulting new chemical properties can be used for quantification or separation of the educt.
What is derivatization reagent?
Derivatization is a technique that usually involves a reaction of the analyte(s) of interest with a particular derivatization reagent. One of the more commonly used in GC analyses involves a reaction that adds a trimethylsilyl (TMS) functional group to the compound. This is also known as trimethylsilylation.
Why is derivatization important in spectroscopy?
4.1 Chemical derivatization coupled with mass spectrometry The main purpose of derivatization is to increase the sensitivity of detection for methylated cytosines. By doing so, both retention times and separation resolution are raised significantly for the detection of the four types of methylated cytosines.
What is the main reason for derivatizing alcohols and acids before analyzing them on a GC MS?
Derivatization is generally necessary in the analysis by GC of compounds that exhibit low volatility, have poor thermal stability, contain “active” groups that can lead to loss of sample to intermolecular hydrogen bonding or adsorption on the inlet or column, and/or demonstrate poor sensitivity at the detector.
How does derivatization work?
What is GC MS analysis?
Gas Chromatography/Mass Spectrometry, or GC/MS analysis, is an analytical method that combines the features of gas chromatography and mass spectrometry to identify different substances within a sample component matrix. GC/MS analysis is generally considered one of the most accurate analyses available.
How is the silylation power of MSTFA enhanced?
The silylation power of MSTFA can be enhanced by the use of catalysts or additives that scavenge reaction by-products. MSTFA reacts in situ with ammonium iodide (NH 4 I) to produce trimethyliodosilane (TMSI), a powerful trimethylsilyl donor. 5
How is diethyl disulphide used in the MSTFA reaction?
In order to prevent iodine incorporation into the product, ethanethiol is added to reduce the formed iodine to hydrogen iodide. As a result, diethyl disulphide is produced during the derivatization reaction. Imidazole acts as a base catalyst in the MSTFA silylation reaction.
How does MSTFA react with ammonium iodide?
MSTFA reacts in situ with ammonium iodide (NH 4 I) to produce trimethyliodosilane (TMSI), a powerful trimethylsilyl donor. 5 In order to prevent iodine incorporation into the product, ethanethiol is added to reduce the formed iodine to hydrogen iodide. As a result, diethyl disulphide is produced during the derivatization reaction.
What happens when MSTFA reacts with ezetimibe?
In this derivatization reaction, MSTFA reacts with labile hydroxyl group of ezetimibe, and the hydroxyl groups are then converted into TMS–ether derivatives under trimethylsilylation derivatization conditions.