Separation of structurally related primary aliphatic amines using hydrophilic interaction chromatography with fluorescence detection after postcolumn derivatization with o -phthaldialdehyde/mercaptoethanol

2017 ◽  
Vol 40 (24) ◽  
pp. 4689-4699 ◽  
Author(s):  
Michal Douša ◽  
Jan Doubský
Keyword(s):  
Fluorescence Detection ◽  
Hydrophilic Interaction Chromatography ◽  
Aliphatic Amines ◽  
Hydrophilic Interaction ◽  
Primary Aliphatic Amines ◽  
Postcolumn Derivatization

scholarly journals Single-Laboratory Validation for the Determination of Cocoa Flavanols and Procyanidins (by Degree of Polymerization DP1–7) in Cocoa-Based Products by Hydrophilic Interaction Chromatography Coupled with Fluorescence Detection: First Action 2020.05

2020 ◽  
Author(s):  
Ugo Bussy ◽  
Gregory Hewitt ◽  
Yusuf Olanrewaju ◽  
Brian R May ◽  
Nicholas Anderson ◽  
...  
Keyword(s):  
Fluorescence Detection ◽  
Degree Of Polymerization ◽  
Laboratory Method ◽  
Hydrophilic Interaction Chromatography ◽  
Hydrophilic Interaction ◽  
Wide Range ◽  
Fit For Purpose ◽  
Single Laboratory ◽  
Cocoa Flavanols

Abstract Background Flavanols and procyanidins are complex bioactives found in many foods such as cocoa. As their consumption is associated with health benefits, cocoa flavanols and procyanidins are receiving increasing attention from consumers, industry, researchers, and regulators. Objective The objective of this study is to validate a method using hydrophilic interaction chromatography (HILIC) with fluorescence detection (FLD) and a commercially available reference material for the determination of flavanols and procyanidins (CF) in cocoa-based products. Methods Method performances were evaluated for cocoa matrices with CF content that ranged from 0.8 to 500 mg/g, which included low CF matrices (milk and dark chocolate, cocoa powder, and liquor) and high CF matrices (cocoa extract and dietary supplement products). The method was validated in a single-laboratory by determining sensitivity, selectivity, linearity, stability, robustness, accuracy, and precision for each of the matrices. Results The method was validated for cocoa matrices with CF content that ranged from 0.8 to 500 mg/g. Accuracy ranged from 86 to 99% and repeatability (RSDr) from 1.5 to 8.6% for CF. Conclusions Analytical performances acquired through this single-laboratory validation study for a wide range of cocoa-based matrices demonstrate that this method is fit-for-purpose for the determination of flavanols and procyanidins in cocoa-based products. Highlights Hydrophilic interaction chromatography (HILIC) with fluorescence detection was successfully used to determine total CF content in multiple product types. Single-laboratory method validation results demonstrate that the method is fit for purpose for cocoa-based matrices containing <0.8 to 500 mg/g of CF.

Exogenous Directing Group Free, Ligand-Enabled gamma-C(sp3)–H Arylation of Free Primary Aliphatic Amines and α-Amino Esters

2019 ◽  
Author(s):  
Yongzheng Ding ◽  
Shuai Fan ◽  
Xiaoxi Chen ◽  
yuzhen gao ◽  
Gang Li
Keyword(s):  
Amino Acids ◽  
Large Scale ◽  
Free Ligand ◽  
Aliphatic Amines ◽  
Rapid Synthesis ◽  
Amino Esters ◽  
Directing Group ◽  
Large Scale Synthesis ◽  
Primary Aliphatic Amines

A Pdᴵᴵ-catalyzed, ligand-enabled gamma-C(sp3)–H arylation of free primary aliphatic amines and amino esters without using an exogenous directing group is reported. This reaction is compatible with unhindered free aliphatic amines, and it is also be applicable to the rapid synthesis of biologically and synthetically valuable unnatural α-amino acids. Large scale synthesis is also feasible using this method.<br>

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