Solid Phase Extraction Purification of Carboxylic Acid Products from 96-Well Format Solution Phase Synthesis with DOWEX 1×8-400 Formate Anion Exchange Resin

2001 ◽  
Vol 3 (2) ◽  
pp. 205-215 ◽  
Author(s):  
Brett C. Bookser ◽  
Shirong Zhu
2016 ◽  
Vol 721 ◽  
pp. 82-86 ◽  
Author(s):  
Kristine Meile ◽  
Aivars Zhurinsh

Automated preparative scale solid phase extraction (SPE) has been used to separate levoglucosan – a valuable platform chemical from the liquid products of wood pyrolysis. The sorbent for SPE was a strongly basic anion exchange resin in OH-form. Separation of levoglucosan could be done with water as the eluent, the regeneration of the resin was done with a NaCl solution. Up-scaling the purification of levoglucosan is a step forward industrial production of this chemical.


2019 ◽  
Vol 91 (7) ◽  
pp. 1243-1255 ◽  
Author(s):  
Victoria R. Kohout ◽  
Alyssa L. Pirinelli ◽  
Nicola L. B. Pohl

Abstract Carbohydrate structures are often complex. Unfortunately, synthesis of the range of sugar combinations precludes the use of a single coupling protocol or set of reagents. Adapting known, reliable bench-chemistry reactions to work via automation will help forward the goal of synthesizing a broad range of glycans. Herein, the preparation of di- and tri-saccharides of alpha 1→2 rhamnan fragments is demonstrated using thioglycoside donors with the development for a solution-phase-based automation platform of commonly used activation conditions using N-iodosuccinimide (NIS) with trimethylsilyl triflate. Byproducts of the glycosylation reaction are shown to be compatible with hydrazine-based deprotection conditions, lending broader functionality to this method as only one fluorous-solid-phase extraction step per coupling/deprotection cycle is required.


Author(s):  
Heesung Moon ◽  
Jiwon Park ◽  
Jinwoo Hwang ◽  
Heesun Chung

Abstract Carbon nanotubes (CNT) are useful for extracting chemical compounds due to their properties, such as surface area and the potential for chemical modification. Especially the formation of carbon nanotubes with carboxylic acid functional group makes them disperse in water-based samples and have strong interaction forces with cationizable analytes. Based on these features, carboxylic acid functionalized multi-walled carbon nanotubes (COOH-MWCNTs) have been used as extraction sorbents. CNT also can be gathered using an external magnet by forming complex with iron oxide (Fe3O4) magnetic nanoparticles (MNPs). In this study, COOH-MWCNTs with MNPs were subjected to magnetic solid phase extraction (mSPE) in order to extract the targeted substances such as diphenhydramine, doxylamine, tramadol, escitalopram, zolpidem, diphenamid, paclobutrazol, hexaconazole, cyproconazole, and mepronil from human plasma samples. The following five factors were optimized: [1] the ratio of COOH-MWCNTs to MNPs as a sorbent from 1: 1 to 1: 4; [2] sorbent amount starting from 12.5% to 75%; [3] sample pH tested pH 2 to pH 10 with 1 N hydrochloride and 1 N sodium hydroxide; [4] agitating time from 0 min to 4 min; [5] elution solvent. LOD of 10 targeted substances in human plasma were in the range of 0.1 to 0.4 mg/L. The recovery of targeted substances (except diphenamid) in human plasma was 73.06–110.28% for intra-day, 83.00–107.70% for inter-day and the precision (RSD, %) in human plasma was 0.3–13.3% for intra-day, 2.9–15.6%. The method was applied to 9 authentic biological samples from overdose patients in the emergency room of Chung-nam National University Hospital. The performance of mSPE was compared with the liquid–liquid extraction (LLE) method using ethyl acetate. The results showed that the newly developed method in this study can be used for screening analysis in forensic and clinical toxicology.


1997 ◽  
Vol 786 (2) ◽  
pp. 259-268 ◽  
Author(s):  
Dianna L. Ambrose ◽  
James S. Fritz ◽  
Michael R. Buchmeiser ◽  
Norbert Atzl ◽  
Günther K. Bonn

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