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A chromatographic procedure for Rb, K, Ba and Sr one-by-one separation from geological materials has been developed by using a single column with packing Sr-spec resin, followed by high-precision Rb isotope measurement by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). The main matrix elements (Ti, Al, Mg, Fe, Mn, Na and Ca) were removed with 4.4 mL of 3 M HNO3 first; Rb and K were then sequentially eluted in different volumes with the same acid. After that, Ba was eluted with 8 M HNO3, and finally Sr was eluted with Milli-Q water. This procedure enables us to collect pure Rb, K, Ba and Sr one by one in a single column with recovery close to 100%. The purified Rb was measured by using a standard-sample bracketing method via MC-ICP-MS. The short-term precision for δ87Rb was better than ±0.03‰ (2SD, for 15 hours), and the long-term (more than 12 months) external precision was better than ±0.06‰ (2SD) based on repeated analysis of Rb standard solution NIST SRM 984. Matrix effects on Rb isotope measurement by MC-ICP-MS were tested by doping pure Rb standard with various amounts of matrix elements and were found to be insignificant when Na/Rb ＜ 2, Ca/Rb ＜ 4 and K/Rb ＜ 25. We measured a set of geological reference standards by this method and found significant Rb isotopic variation. Our study suggests that Rb isotope geochemistry may be a promising tracer of various cosmochemical and geological processes. [ABSTRACT FROM AUTHOR]

Given recent advances in automated oligosaccharide synthesis, analytical techniques that can be coupled to a synthetic framework are needed to not just identify but also purify to homogeneity protected carbohydrate compounds at levels of ≥99.5% purity. Herein, an alternate-pump recycling high-performance liquid chromatography (R-HPLC) method has been developed to allow purification of protected carbohydrates at levels of ≥99.5% purity. [ABSTRACT FROM AUTHOR]

The present paper discusses a comparative study concerning performance efficiency and sustainable impact of three purification processes for degenotoxification of Active Pharmaceutical Ingredients (APIs) post reaction streams: recrystallization, flash chromatography and organic solvent nanofiltration (OSN). Two case studies in each process were selected for evaluation of the separation technologies featuring the same model API being Mometasone furoate (Meta) glucocorticoid and two genotoxic impurities (GTIs). Methyl mesylate (MeMS) and 4-dimethylaminopyridine (DMAP) were chosen as model impurities due to their incidental appearance in glucocorticoids based on a common methanesulfonylation manufacturing step. Successful degenotoxification was achieved in all cases concerning DMAP and MeMS reaching final GTI levels below the regulatory thresholds with the exception of DMAP using recrystallization. API losses were 5% and 6.4% for OSN, 6.4% and 11.9% for flash chromatography and 14.9% and 16.4% for recrystallization during the removal of DMAP and MeMS, respectively. The API loss occurring during the purification processes has a significant impact on the outcome of cost analysis. Mass and carbon intensity values are highest for OSN and lowest for recrystallization, while flash chromatography has intermediate values. Although recrystallization is more time consuming, it should not be discarded without careful analysis since API loss often declines at larger scales and it generally gives the API in the desired crystallographic form. Solvent recycling has a significant impact on the sustainability of all the processes by the reduction of mass intensity by two orders of magnitude (from 400–1300 to 14–63 kg/kg-API, depending on the process) and narrowing down carbon intensity to the range of 100–200 kg-CO2/kg-API. OSN requires the use of 7 diavolumes, therefore its high performance is achieved at the cost of high solvent usage. Hence, solvent recycling also has a higher positive environmental impact on OSN. [ABSTRACT FROM AUTHOR]

Replacement of dichloromethane as the bulk medium within chromatographic purification has been evaluated with a broad range of molecules containing functionality common within Medicinal Chemistry programmes. Analysis of the data set has generated a set of general guidelines to assist in the selection of alternative solvents for CH2Cl2 as the bulk media in these ubiquitously employed processes. [ABSTRACT FROM AUTHOR]

New regio- and chemoselective [4+2+1] domino cyclization consisting of the formation of two spiro rings and five σ bonds has been developed for the synthesis of spiro-substituted benzo[b]furo[3,4-e][1,4]diazepine derivatives. The reaction is a multicomponent domino green process and can be readily performed by reacting inexpensive starting materials of benzene-1,2-diamines, tetronic acid and 2,2-dihydroxy-2H-indene-1,3-dione in aqueous solution under microwave irradiation. The present synthesis shows attractive characteristics, such as the use of water as reaction media, convenient one-pot operation, short reaction periods of 10–18 min and reduced waste production without the use of any strong acids or metal promoters. This synthesis serves as a nice addition to GAP (Group-Assistant-Purification) chemistry in which purification viachromatography and recrystallization can be avoided, and the pure products were obtained simply by washing the crude products with 95% EtOH. [ABSTRACT FROM AUTHOR]