Development and Validation of 2-Azaspiro [4,5] Decan-3-One (Impurity A) in Gabapentin Determination Method Using qNMR Spectroscopy |
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| Authors: | Nataliya E Kuz&#x;mina Sergey V Moiseev Mikhail D Khorolskiy Anna I Lutceva |
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| Institution: | 1.“Scientific Centre for Expert Evaluation of Medicinal Products” of the Ministry of Health of the Russian Federation, Federal State Budgetary Institution, 8/2 Petrovsky Blvd, 127051 Moscow, Russia; (S.V.M.); (M.D.K.); (A.I.L.);2.Department of Pharmaceutical and Toxicological Chemistry Named by A.P. Arzamastsev, I.M. Sechenov First Moscow State Medical University (Sechenov University), 8, Bldg. 2 St. Trubetskaya, 119991 Moscow, Russia |
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| Abstract: | The authors developed a 1H qNMR test procedure for identification and quantification of impurity A present in gabapentin active pharmaceutical ingredient (API) and gabapentin products. The validation studies helped to determine the limit of quantitation and assess linearity, accuracy, repeatability, intermediate precision, specificity, and robustness of the procedure. Spike-and-recovery assays were used to calculate standard deviations, coefficients of variation, confidence intervals, bias, Fisher’s F test, and Student’s t-test for assay results. The obtained statistical values satisfy the acceptance criteria for the validation parameters. The authors compared the results of impurity A quantification in gabapentin APIs and capsules by using the 1H qNMR and HPLC test methods. |
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| Keywords: | gabapentin impurity A validation limit of the quantitation linearity accuracy repeatability precision specificity robustness qNMR HPLC |
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