Retrospective review of methodological foundations for the new monograph «Spectrometry in the near infrared regioN»

The new pharmacopoeial monograph «Spectrometry in the near infrared region» reflects the results of a difficult path traversed from the development of measurement and analytical techniques to the introduction of NIR spectroscopy in the practice of quality control. This review discusses the new monograph of the XIII edition of the State Pharmacopoeia in the light of existing methodological approaches developed and validated for the assessment of drug quality parameters such as identification, content uniformity, assay, etc. Special attention is paid to the formation of spectral libraries - the factor of the sample’s «age» is considered as a source of additional spectral variability. The review raises the question of the NIR spectra identity criteria. Drawing on the example of techniques developed for the evaluation of batch variability (23 medicines) it was showed that obtained values of spectral range serve as unique characteristics of each individual product and production process, defining interlot reproducibility - the less the spectral distance between the series is, the more homogeneous the products are. NIR spectroscopy was shown to be effective for quantitative analysis of solid dosage forms and liquid substances. The authors considered the principles of operation as well as prospects for the practical use of the new technology - NIR chemical imaging, combining spectral analysis and digital image.

спектроскопия в ближней инфракрасной области, контроль качества лекарственных средств, государственная фармакопея, методики идентификации и количественного анализа, БИК-визуализация, spectroscopy in the near infrared region, quality control of medicines, State Pharmacopoeia, identification and assay methods, NIR imaging

1. Elizarova TE, Morozova MA, Pleteneva TV. Change in time of spectral characteristics of drug substances (NIR region). Vestnik RUDN (series of Medical science) 2011; (3): 153–7 (in Russian).

2. Yakushev VA, Morozova MA, Elizarova TE, Fitilev SB, Pleteneva TV. Methods for the protection against counterfeit medications. Part 2. The assessment of interlot dispersion of the metroprolol succinate tablets fabricated by differet manufacturers. Sudebno-meditsinskaya ekspertiza 2012; (5): 46–48 (in Russian).

3. Morozova MA, Elizarova TE, Pleteneva TV. Discriminant analysis and Mahalanobis distance (NIR diffuse reflectance spectra) in the assessment of drug’s batch-to- batch dispersion and quality threshold establishment. European Scientific journal 2013; 9(25): 8–25.

4. Ritchie GE, Mark H, Ciurczak EW. Evaluation of the Conformity Index and the Mahalanobis Distance as a Tool for Process Analysis: A Technical Note. AAPS Pharm. Sci. Tech. 2003; 4(2): 109–18.

5. Gemperline PJ, Boyer NR. Classification of Near-Infrared Spectra Using Wavelength Distances: Comparison to the Mahalanobis Distance and Residual Variance Methods. Anal. Chem. 1995; 67: 160–6.

6. De Maesschalck R, Jouan-Rimbaud D, Massart DL. The Mahalanobis distance. Chemom Intellig Lab Syst. 2000; 50: 1–18.

7. Mark HL, Tunnell D. Qualitative near-infrared reflectance analysis using Mahalanobis distances. Anal. Chem. 1985; 57: 1449–56.

8. Whitfield RG, Gerger ME, Sharp RL. Near-infrared spectrum qualification via Mahalanobis distance determination. J. Appl. Spectros. 1987; 41: 1204–13.

9. Andre M. Multivariate Analysis and Classification of the Chemical Quality of 7- aminocephalosporanic Acid Using Near-Infrared Reflectance Spectroscopy. Anal. Chem. 2003; 75: 3460–7.

10. Märk J, Andre M, Karner M, Huck CW. Prospects for multivariate classification of a pharmaceutical intermediate with near-infrared spectroscopy as a process analytical technology (PAT) production control supplement. Eur. J. Pharm. Biopharm. 2010; 76: 320–7.

11. Elizarova TE, Morozova MA, Pleteneva TV. Possibility of using near-IR spectrometry for drug quality control with respect to dose uniformity. Pharmaceutical Chemistry Journal 2011; 45(5): 302–5.

12. Gowen AA, O’Donnell CP, Cullen PJ, Bell SE. Recent applications of Chemical Imaging to pharmaceutical process monitoring and quality control. Eur. J. Pharm. Biopharm. 2008; 69(1), 10–22.

13. Salzer R, Siesler HW. Infrared and Raman Spectroscopic Imaging. Wiley-VCH; 2009.

14. Franch-Lage F, Amigo Rubio JM, Skibsted E, Maspoch S, Coello J. Quantitative determination of api and excipients in lorazepam tablets by using NIR-hyperspectral image and MCR-ALS. Paper presented at 7th Colloquium Chemiometricum Mediterraneun (CCM VII 2010 — Granada). Granada, Spain; 2010.

15. Dorofeeva ND, Bazarkina OV, Pleteneva TV, Gordeeva MA, Elizarova TE. Pharmacoeconomic evaluation of the effectiveness of NIR method. Novaya apteka: effektivnoe upravlenie 2010; (12): 39–42 (in Russian).