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Supercritical CO2 elimination of solvent residues from active pharmaceutical ingredients: Beclometasone dipropionate and Budesonide
The Journal of Supercritical Fluids ( IF 3.4 ) Pub Date : 2021-06-24 , DOI: 10.1016/j.supflu.2021.105325
Lucia Baldino , Mariarosa Scognamiglio , Ernesto Reverchon

The scope of this work was to reduce/eliminate Class 2 and Class 3 solvents, contained in two active pharmaceutical ingredients (APIs), Beclometasone dipropionate (Beclo) and Budesonide (Bude), using supercritical CO2. The process was carried out at pressures from 80 to 370 bar, CO2 flow rates between 0.1 and 1.0 kg/h, and at a temperature of 40 °C. When CO2 density was too low (e.g., at 80 bar and 40 °C), an incomplete extraction of the solvents was obtained. When the extraction pressure was too large (e.g., 370 bar), also a non-negligible co-extraction of solid material was observed. Particles bed caking emerged at CO2 flow rates larger than 0.7 kg/h. The optimal process conditions were found operating at 200 bar and 40 °C, using a 0.7 kg/h CO2 flow rate: total final solvent residues of 5 ppm and 52 ppm for Beclo and Bude, respectively, were reached.



中文翻译:

超临界 CO 2去除活性药物成分中的溶剂残留:二丙酸倍氯米松和布地奈德

这项工作的范围是使用超临界 CO 2减少/消除包含在两种活性药物成分 (API),二丙酸倍氯米松 (Beclo) 和布地奈德 (Bude) 中的第 2 类和第 3 类溶剂。该过程在 80 至 370 巴的压力、0.1 至 1.0 kg/h 的CO 2流速和 40 °C 的温度下进行。当 CO 2密度过低(例如,在 80 bar 和 40 °C 下)时,溶剂的萃取不完全。当萃取压力太大(例如,370 巴)时,也观察到不可忽略的固体材料共萃取。CO 2 下出现颗粒床结块流速大于 0.7 kg/h。发现最佳工艺条件在 200 bar 和 40 °C 下运行,使用 0.7 kg/h CO 2流速:Beclo 和 Bude 的最终溶剂残留总量分别达到 5 ppm 和 52 ppm。

更新日期:2021-06-30
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