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一种简单、绿色的液质联用色谱法,用于测定含牛奶的模拟胃肠介质中的布洛芬,以监测三维打印制剂的溶出研究。

A simple and green liquid chromatography method for the determination of ibuprofen in milk-containing simulated gastrointestinal media for monitoring the dissolution studies of three-dimensional-printed formulations.

机构信息

Department of Pharmaceutical Technology, Laboratory of Pharmaceutical Analysis, School of Pharmacy, Aristotle University of Thessaloniki, Thessaloniki, Greece.

Department of Chemistry, Laboratory of Analytical Chemistry, Faculty of Sciences, Aristotle University of Thessaloniki, Thessaloniki, Greece.

出版信息

J Sep Sci. 2022 Nov;45(21):3955-3965. doi: 10.1002/jssc.202200444. Epub 2022 Sep 8.

DOI:10.1002/jssc.202200444
PMID:36054076
Abstract

A fast and green ultra-high-performance liquid chromatographic method was developed for the determination of ibuprofen in milk-containing simulated gastrointestinal media to monitor the dissolution of three-dimensional printed formulations. To remove interfering compounds, protein precipitation using methanol as a precipitation reagent was performed. The separation of the target analyte was performed on a C column using a mobile phase consisting of 0.05% v/v aqueous phosphoric acid solution: methanol, 25:75% v/v. Method validation was conducted using the total error concept. The β-expectation tolerance intervals did not exceed the acceptance criteria of ±15%, meaning that 95% of future results will be included in the defined bias limits. The relative bias ranged between ─1.1 and +3.2% for all analytes, while the relative standard deviation values for repeatability and intermediate precision were less than 2.8% and 3.9%, respectively. The achieved limit of detection was 0.01 μg/ml and the lower limit of quantitation was established as 2 μg/ml. The proposed method was simple, and it required reduced organic solvent consumption following the requirements of Green Analytical Chemistry. The method was successfully employed for the determination of ibuprofen in real biorelevant media obtained from dissolution studies.

摘要

建立了一种快速、绿色的超高效液相色谱法,用于测定含乳模拟胃肠介质中的布洛芬,以监测三维打印制剂的溶出度。为了去除干扰化合物,采用甲醇作为沉淀试剂进行蛋白质沉淀。采用 0.05%(v/v)磷酸水溶液:甲醇,25:75%(v/v)作为流动相,在 C 柱上进行目标分析物的分离。采用总误差概念进行方法验证。β-期望容忍区间不超过±15%的验收标准,这意味着 95%的未来结果将包含在定义的偏差限值内。所有分析物的相对偏差均在-1.1%至+3.2%之间,而重复性和中间精密度的相对标准偏差值分别小于 2.8%和 3.9%。所达到的检测限为 0.01μg/ml,定量下限定为 2μg/ml。该方法简单,符合绿色分析化学的要求,有机溶剂消耗减少。该方法成功地用于测定溶解研究中从真实生物相关介质中获得的布洛芬。

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