Column chromatography is a technique widely used for the purification of active pharmaceutical ingredients (APIs). One of the common solvent systems used by this technique is blends of dichloromethane (DCM) and methanol (MeOH), thereby exposing workers to health and safety risks and making the pharmaceutical sector one of the major contributors to chlorinated solvent waste. In this work, API separation and purification using several alternative safer solvent blends in column chromatography were evaluated and compared to DCM/MeOH. Ibuprofen and acetaminophen were used as model APIs, and caffeine was used as a model additive. Overall, some of the safer solvent blends tested provided better performance, with higher API recovery and purity compared to DCM/MeOH, in addition to potential health, safety, and environmental benefits. Specifically, blends of heptane/ethyl acetate and heptane/methyl acetate showed the most promise. Our work demonstrates the potential of these safer solvent blends as possible replacements for DCM/MeOH in API purification, thereby addressing a critical safety concern in the pharmaceutical industry.
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http://dx.doi.org/10.1021/acsenvironau.4c00015 | DOI Listing |
J Chromatogr B Analyt Technol Biomed Life Sci
December 2024
United States Army Medical Research Institute of Chemical Defense, 8350 Ricketts Point Road, Aberdeen Proving Ground, MD 21010, USA. Electronic address:
Chemical warfare nerve agents (CWNAs) are potent and irreversible inhibitors of acetylcholinesterase (AChE). Oxime reactivators are an important part of the standard treatment for CWNA exposure as they can reactivate inhibited AChE. Evaluating the oxime candidates of interest in biological samples requires analytical detection methods and oxime reactivators as a class of compounds have historically been notoriously difficult to isolate, detect and analyze in an analytical laboratory, and there are currently no sensitive or robust analytical detection methods in the literature.
View Article and Find Full Text PDFJ Chromatogr B Analyt Technol Biomed Life Sci
December 2024
Department of Chromatography, Institute of Chemical Sciences, Faculty of Chemistry, Maria Curie Sklodowska University in Lublin, 20-031 Lublin, Poland. Electronic address:
Solid phase extraction (SPE) is one of the most popular methods of preparing plasma samples before determining the xenobiotics they contain. The present paper shows that the recovery degree of xenobiotics from plasma samples using SPE with C18 sorbent strongly depends on their storage time and temperature. While xenobiotics can be isolated and recovered in 100 % from fresh plasma samples under optimal conditions of the SPE procedure, their SPE recovery degree from stored plasma is lower.
View Article and Find Full Text PDFJ Chromatogr A
December 2024
I. U. CINQUIMA, Analytical Chemistry Group (TESEA), Dept. Analytical Chemistry, Faculty of Sciences, University of Valladolid 47011, Valladolid, Spain. Electronic address:
The simultaneous separation of the enantiomers of six anticoagulant rodenticides, derived from 4-hydroxycoumarin, has been studied in this work. Ten different stationary phases (zwitterionic, Pirkle-type, polysaccharides and macrocyclic antibiotics derivatives) were evaluated by using supercritical fluid chromatography coupled to two different detectors (circular dichroism and mass spectrometry-single quadrupole). The effect of the type of organic modifier and temperature on the chiral separation was investigated, and the best results were obtained with the column Regis S,S-Whelk-O1 at 25 °C when using a gradient elution program with methanol as organic modifier.
View Article and Find Full Text PDFJ Chromatogr A
December 2024
Department of Chemistry, Wayne State University, Detroit, MI 48202, USA.
Reversed-phase liquid chromatography (RPLC) offers significant advantages over traditional methods for estimating octanol-water partition constants, which are a critical parameter in drug discovery. In contrast to classical methods for determining the octanol-water partition constant, such as shake-flask techniques, RPLC is less time-consuming and easier to automate. In this study, we explored three alternative organic solvent modifiers: acetone, 2-propanol, and tetrahydrofuran for the indirect determination of the octanol-water partition constant for neutral compounds by RPLC using either isocratic retention factors or retention factors extrapolated to 100 % water for several stationary phases.
View Article and Find Full Text PDFJ Pharm Biomed Anal
December 2024
State Key Laboratory of Chinese Medicine Modernization, Tianjin University of Traditional Chinese Medicine, Tianjin 301617, China. Electronic address:
The medicinal fungus Phellinus Igniarius (P. igniarius) has been demonstrated to possess a variety of pharmacological effects, including anti-oxidant, anti-tumor, blood circulation promotion, anti-diarrheal and sedative properties, etc. In order to gain a deeper understanding of the components in P.
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