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使用传统和环保型稳定性指示高效薄层色谱法对泊马度胺进行定量分析:验证参数对比

Quantification of Pomalidomide Using Conventional and Eco-Friendly Stability-Indicating HPTLC Assays: A Contrast of Validation Parameters.

作者信息

Alam Prawez, Shakeel Faiyaz, Iqbal Muzaffar, Foudah Ahmed I, Alqarni Mohammed H, Aljarba Tariq M, Abdel Bar Fatma, Alshehri Sultan

机构信息

Department of Pharmacognosy, College of Pharmacy, Prince Sattam Bin Abdulaziz University, Al-Kharj 11942, Saudi Arabia.

Department of Pharmaceutics, College of Pharmacy, King Saud University, Riyadh 11451, Saudi Arabia.

出版信息

ACS Omega. 2023 Aug 7;8(33):30655-30664. doi: 10.1021/acsomega.3c04382. eCollection 2023 Aug 22.

Abstract

High-performance thin-layer chromatographic (HPTLC) assays for pomalidomide (PMD) measurement are lacking in the published database. Furthermore, eco-friendly stability-indicating analytical assays for PMD measurement are also lacking in the published database. In order to detect PMD in commercial products more accurately and sustainably than the conventional normal-phase HPTLC (NP-HPTLC) assay, an effort was made to design and verify a sensitive and eco-friendly reversed-phase HPTLC (RP-HPTLC) assay. The silica gel 60 NP-18F254S and 60 RP-18F254S plates were used as the stationary phases for NP-HPTLC and RP-HPTLC methods, respectively. The solvent system for NP-HPTLC was chloroform-methanol (90:10 v/v). However, the solvent system for RP-HPTLC was ethanol-water (75:25 v/v). The greenness scores for both assays were measured by AGREE approach. PMD measurement was performed for both assays at 372 nm. In the 50-600 and 20-1000 ng/band ranges, the NP-HPTLC and RP-HPTLC methods were linear for PMD measurement. The RP-HPTLC assay was superior to the NP-HPTLC method for measuring PMD in terms of sensitivity, accuracy, precision, and robustness. The ability of both methods to identify PMD in the presence of its degradation products suggests that both methods have stability-indicating features. When employing the NP-HPTLC and RP-HPTLC assays, respectively, the assay for PMD in commercial capsules was 88.68 and 98.83%. The AGREE scores for NP-HPTLC and RP-HPTLC assays were calculated to be 0.44 and 0.82, respectively, suggesting an outstanding greenness characteristic of the RP-HPTLC method than the NP-HPTLC method. The RP-HPTLC method was found to be superior to the NP-HPTLC method based on these findings. Therefore, the RP-HPTLC method could be successfully applied for the determination of PMD in pharmaceutical products.

摘要

已发表的数据库中缺乏用于测定泊马度胺(PMD)的高效薄层色谱(HPTLC)分析方法。此外,已发表的数据库中也缺乏用于测定PMD的环保型稳定性指示分析方法。为了比传统的正相HPTLC(NP-HPTLC)分析方法更准确、更可持续地检测商业产品中的PMD,人们努力设计并验证了一种灵敏且环保的反相HPTLC(RP-HPTLC)分析方法。硅胶60 NP-18F254S板和60 RP-18F254S板分别用作NP-HPTLC和RP-HPTLC方法的固定相。NP-HPTLC的溶剂系统是氯仿 - 甲醇(90:10 v/v)。然而,RP-HPTLC的溶剂系统是乙醇 - 水(75:25 v/v)。两种分析方法的绿色度评分通过AGREE方法测定。两种分析方法均在372 nm处进行PMD测定。在50 - 600和20 - 1000 ng/条带范围内,NP-HPTLC和RP-HPTLC方法用于PMD测定呈线性。在灵敏度、准确度、精密度和稳健性方面,RP-HPTLC分析方法在测定PMD方面优于NP-HPTLC方法。两种方法在其降解产物存在下鉴定PMD的能力表明两种方法都具有稳定性指示特征。分别采用NP-HPTLC和RP-HPTLC分析方法时,商业胶囊中PMD的测定结果分别为88.68%和98.83%。计算得出NP-HPTLC和RP-HPTLC分析方法的AGREE评分分别为0.44和0.82,表明RP-HPTLC方法比NP-HPTLC方法具有更突出的绿色度特征。基于这些发现,RP-HPTLC方法被发现优于NP-HPTLC方法。因此,RP-HPTLC方法可成功应用于药品中PMD的测定。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/0e26/10448633/498beab25e04/ao3c04382_0002.jpg

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