Method development and validation for pharmaceutical tablets analysis using transmission Raman spectroscopy

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• 作者：Yi Li^a ; Benoî ; t Igne^b ; James K. Drennen III^a ; ^b ; Carl A. Anderson^a ; ^b ; ^{andersonca@duq.edu" class="auth_mail" title="E-mail the corresponding author}
• 关键词：Transmission Raman spectroscopy ; Validation ; ICH-Q2 ; Stability-indicating assay
• 刊名：International Journal of Pharmaceutics
• 出版年：2016
• 出版时间：10 February 2016
• 年：2016
• 卷：498
• 期：1-2
• 页码：318-325
• 全文大小：1646 K

文摘

The objective of the study is to demonstrate the development and validation of a transmission Raman spectroscopic method using the ICH-Q2 Guidance as a template. Specifically, Raman spectroscopy was used to determine niacinamide content in tablet cores. A 3-level, 2-factor full factorial design was utilized to generate a partial least-squares model for active pharmaceutical ingredient quantification. Validation of the transmission Raman model was focused on figures of merit from three independent batches manufactured at pilot scale. The resultant model statistics were evaluated along with the linearity, accuracy, precision and robustness assessments. Method specificity was demonstrated by accurate determination of niacinamide in the presence of niacin (an expected related substance). The method was demonstrated as fit for purpose and had the desirable characteristics of very short analysis times (∼2.5s per tablet). The resulting method was used for routine content uniformity analysis of single dosage units in a stability study.