pharmjournalРазработка и регистрация лекарственных средствDrug development & registration2305-20662658-5049LLC «CPHA»10.33380/2305-2066-2020-9-3-129-136pharmjournal-815Research ArticleМЕТОДЫ АНАЛИЗА ЛЕКАРСТВЕННЫХ СРЕДСТВANALYTICAL METHODSВалидация хроматографических методик: контроль чистоты пиков и специфичности методик с использованием диодно-матричных детекторов (обзор)Validation of Chromatographic Methods: Checking the Peak Purity and the Specificity of Methods with Diode Array Detectors (Review)https://orcid.org/0000-0001-8047-4078ЭпштейнН. А.EpshteinN. A.

Эпштейн Наум Аронович - заведующий лабораторией.

115446, Москва, Коломенский проезд, д. 13А.

Naum A. Epshtein.

13A, Kolomensky proezd, Moscow, 115446.

naumepshtein@gmail.comДепартамент регистрации и разработки лекарственных средств ООО «ИРВИН 2»Department of registration and development of medicines LLC «IRVIN 2»20200207202093129136Copyright © Эпштейн Н.А., 20202020Эпштейн Н.А.Epshtein N.A.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://www.pharmjournal.ru/jour/article/view/815Введение

Введение. При разработке и валидации методик определения примесей важно тестировать спектральную чистоту пиков (SPP) основных веществ с помощью диодно-матричных детекторов (DAD).

Текст

Текст. Подчеркнуто, что задачей тестирования SPP является обнаружение незаметных коэлюирующихся примесей под пиком основного вещества, а не контроль абсолютной чистоты пика. Тестирование SPP снижает риск получения недостаточно специфичной методики. В связи с этим рассмотрены основные критерии и ключевые моменты для оценки спектральной чистоты пиков при использовании компьютерных программ хроматографов Agilent, Shimadzu и Waters.

Заключение

Заключение. Даны рекомендации, которые следует учитывать для корректной оценки спектральной чистоты пиков при разработке хроматографических методик и валидации их специфичности.

Introduction

Introduction. When developing and validating methods of impurity determination, it is important to test the spectral peak purity (SPP) of the main substances using diode array detectors (DAD).

Text

Text. It is emphasized that the task of testing SPP is to detect invisible coeluting impurities under the peak of the main substance, and not the control the absolute purity of the peak. SPP testing reduces the risk of getting non enough specific methods. In this regard, we considered the main criteria and key points for assessing the spectral purity of peaks when using computer programs of Agilent's, Shimadzu's, and Waters's chromatographs.

Conclusion

Conclusion. Recommendations are given, which should be taken into account for the correct assessment of spectral purity of peaks during development of chromatographic methods and validation of their specificity.

чистота пикадиодно-матричный детекторжидкостная хроматографияпримесиAgilentShimadzuWaterspeak puritydiode array detectorliquid chromatographyimpuritiesAgilentShimadzuWatersReferencesICH Harmonised Tripartite Guideline. Validation of Analytical Procedures: Text and Methodology Q2(R1). ICH, 2005. 13 p.ICH Harmonised Tripartite Guideline. Validation of Analytical Procedures: Text and Methodology Q2(R1). ICH, 2005. 13 p.United States Pharmacopoeia. <1225> Validation of compendial procedures. USP41-NF36. 2018.United States Pharmacopoeia. <1225> Validation of compendial procedures. USP41-NF36. 2018.Guidance on the validation of analytical methods for testing drugs. EAEU. 2018. 25 с. (In Russ.).Guidance on the validation of analytical methods for testing drugs. EAEU. 2018. 25 с. (In Russ.).Bylund D., Danielsson R., Markides K. E. Peak purity assessment in liquid chromatography-mass spectrometry. J. Chromatography A. 2001;915: 43-52. Doi: https://doi.org/10.1016/S0021-9673(01)00543-X.Bylund D., Danielsson R., Markides K. E. Peak purity assessment in liquid chromatography-mass spectrometry. J. Chromatography A. 2001;915: 43-52. Doi: https://doi.org/10.1016/S0021-9673(01)00543-X.Dyrstad K., Hvattum Er., Jara S., Lie A. Peak-purity by LC-MS and LC-DAD (presentation). 2015.Dyrstad K., Hvattum Er., Jara S., Lie A. Peak-purity by LC-MS and LC-DAD (presentation). 2015.Dong M. W. HPLC and UHPLC for Practicing Scientists, 2<sup>nd</sup> Ed. Hoboken, United States: Wiley. 2019.Dong M. W. HPLC and UHPLC for Practicing Scientists, 2<sup>nd</sup> Ed. Hoboken, United States: Wiley. 2019.Shockcor J. P. HPLC-NMR Pharmaceutical Applications. Du Pont Pharmaceuticals Co. Newark, NJ, USA: Elsevier. 2017. 271 р.Shockcor J. P. HPLC-NMR Pharmaceutical Applications. Du Pont Pharmaceuticals Co. Newark, NJ, USA: Elsevier. 2017. 271 р.Shackman J. G., Kleintop B. L. Peak purity assessment in a tripleactive fixed-dose combination drug product related substances method using a commercial two-dimensional liquid chromatography system. J. Sep. Sci. 2014;37:2688-2695. Doi: https://doi.org/10.1002/jssc.201400515.Shackman J. G., Kleintop B. L. Peak purity assessment in a tripleactive fixed-dose combination drug product related substances method using a commercial two-dimensional liquid chromatography system. J. Sep. Sci. 2014;37:2688-2695. Doi: https://doi.org/10.1002/jssc.201400515.Zhang K., Wang J., Tsang M., Wigman L., Chetwyn N. TwoDimensional HPLC in Pharmaceutical Analysis. Amer. Pharm. Review. 2013;16(7):39-44.Zhang K., Wang J., Tsang M., Wigman L., Chetwyn N. TwoDimensional HPLC in Pharmaceutical Analysis. Amer. Pharm. Review. 2013;16(7):39-44.Polstera J., Sauerwald N., Feucht W., Treutter D. New methods for spectrometric peak purity analysis in chromatography. J. Chromatography A. 1998;800:21-133. Doi: https://doi.org/10.1016/S0021-9673(97)01132-1Polstera J., Sauerwald N., Feucht W., Treutter D. New methods for spectrometric peak purity analysis in chromatography. J. Chromatography A. 1998;800:21-133. Doi: https://doi.org/10.1016/S0021-9673(97)01132-1Levin Sh. Considerations in Peak Purity Measurements (presentation). 1999. 60 p.Levin Sh. Considerations in Peak Purity Measurements (presentation). 1999. 60 p.Stahl M. Peak purity analysis in HPLC and CE using diode-array technology. Application. Waldbronn, Germany: Agilent Technologies. 2003. 16 p.Stahl M. Peak purity analysis in HPLC and CE using diode-array technology. Application. Waldbronn, Germany: Agilent Technologies. 2003. 16 p.Papadoyannis I. N., Gika H. G. Peak Purity Determination with a Diode Array Detector. In Encyclopedia of Chromatography. N.Y.: Marcel Dekker, Inc. 2003.Papadoyannis I. N., Gika H. G. Peak Purity Determination with a Diode Array Detector. In Encyclopedia of Chromatography. N.Y.: Marcel Dekker, Inc. 2003.Rutan S. C., Venkatramani C. J., Stoll D. R. Peak Purity in Liquid Chromatography, Part I: Basic Concepts, Commercial Software, and Limitations. LC-GC North America. 2018;36(2):100-110.Rutan S. C., Venkatramani C. J., Stoll D. R. Peak Purity in Liquid Chromatography, Part I: Basic Concepts, Commercial Software, and Limitations. LC-GC North America. 2018;36(2):100-110.Cook D. W., Rutan S. C., Venkatramani C. J., Stoll D. R. Peak Purity in Liquid Chromatography, Part II: Potential of Curve Resolution Techniques. LC-GC North America. 2018;36(4):248-255.Cook D. W., Rutan S. C., Venkatramani C. J., Stoll D. R. Peak Purity in Liquid Chromatography, Part II: Potential of Curve Resolution Techniques. LC-GC North America. 2018;36(4):248-255.Stoll D. R., Venkatramani C. J., Rutan S. C. Peak Purity in Liquid Chromatography, Part III: Using Two-Dimensional Liquid Chromatography. LC-GC North America. 2018;36(6):356-361.Stoll D. R., Venkatramani C. J., Rutan S. C. Peak Purity in Liquid Chromatography, Part III: Using Two-Dimensional Liquid Chromatography. LC-GC North America. 2018;36(6):356-361.Mas S., de Juan A. Peak Purity and Resolution of Chromatographic Data in Chemometrics in chromatography. Boca Raton: CRC Press. 2018.Mas S., de Juan A. Peak Purity and Resolution of Chromatographic Data in Chemometrics in chromatography. Boca Raton: CRC Press. 2018.Letter W. Peak Purity Determination by HPLC Diode Array Detector (DAD/PDA) based Chromatography Software (Limitations and Uses). Conference «HPLC diode array method development training course» presented at NJ (USA). 1996. Doi: https://doi.org/10.13140/RG.2.2.29067.90409.Letter W. Peak Purity Determination by HPLC Diode Array Detector (DAD/PDA) based Chromatography Software (Limitations and Uses). Conference «HPLC diode array method development training course» presented at NJ (USA). 1996. Doi: https://doi.org/10.13140/RG.2.2.29067.90409.Empower PDA Software Getting Started Guide. Waters Corporation. 2002. 145 р.Empower PDA Software Getting Started Guide. Waters Corporation. 2002. 145 р.Agilent ChemStation for LC 3D Systems Understanding Your Spectra Module. Understanding Your Spectra Module. Agilent Technologies. 2008. 48 р.Agilent ChemStation for LC 3D Systems Understanding Your Spectra Module. Understanding Your Spectra Module. Agilent Technologies. 2008. 48 р.LabSolutions Data Acquisition & Processing Theory Guide. Kyoto: Shimadzu Corporation. 2012. 84 р.LabSolutions Data Acquisition & Processing Theory Guide. Kyoto: Shimadzu Corporation. 2012. 84 р.Tip #134: Working with 3D PDA data in Empower Software (Part 1). Available at: https://blog.waters.com/get-empowered-review-window-and-the-processing-method-tip-134-3d-pda-data.Tip #134: Working with 3D PDA data in Empower Software (Part 1). Available at: https://blog.waters.com/get-empowered-review-window-and-the-processing-method-tip-134-3d-pda-data.Tip #135: Working with 3D PDA data in Empower Software (Part 2). Available at: https://blog.waters.com/get-empowered-review-window-and-the-processing-method-tip-135-3d-pda-data.Tip #135: Working with 3D PDA data in Empower Software (Part 2). Available at: https://blog.waters.com/get-empowered-review-window-and-the-processing-method-tip-135-3d-pda-data.Tip #136: Working with 3D PDA data in Empower Software (Part 3). Available at: https://blog.waters.com/get-empowered-review-window-and-the-processing-method-tip-136-3d-pda-data.Tip #136: Working with 3D PDA data in Empower Software (Part 3). Available at: https://blog.waters.com/get-empowered-review-window-and-the-processing-method-tip-136-3d-pda-data.Tip #137: Working with 3D PDA data in Empower Software (Part 4). Available at: https://blog.waters.com/get-empowered-review-window-and-the-processing-method-tip-137-3d-pda-data.Tip #137: Working with 3D PDA data in Empower Software (Part 4). Available at: https://blog.waters.com/get-empowered-review-window-and-the-processing-method-tip-137-3d-pda-data.How do you set up the Purity Thresholds in Empower 3? Waters Knowledge Base: WKB11215.How do you set up the Purity Thresholds in Empower 3? Waters Knowledge Base: WKB11215.Epshtein N. A. About stress experiments by developing / improving analytical methods and technology of drug substances and medicines. Razrabotka i registratsiya lekarstvennykh sredstv = Drug Development & Registration. 2016;3(16):118-132 (In Russ.).Epshtein N. A. About stress experiments by developing / improving analytical methods and technology of drug substances and medicines. Razrabotka i registratsiya lekarstvennykh sredstv = Drug Development & Registration. 2016;3(16):118-132 (In Russ.).Waters 996 Photodiode Detector: Peak Purity III. Interpretation of peak purity plots. Waters. 1996. Available at: https://www.waters.com/waters/library.htm?locale=en_US&lid=1536113Waters 996 Photodiode Detector: Peak Purity III. Interpretation of peak purity plots. Waters. 1996. Available at: https://www.waters.com/waters/library.htm?locale=en_US&lid=1536113Mito (Shimadzu) Ya. Chromatogram Peak Purity Determination Apparatus. United States patent US 2014/0067283 A1, 2014 Mar. 6. Available at: https://patents.google.com/patent/US20140067283A1/en.Mito (Shimadzu) Ya. Chromatogram Peak Purity Determination Apparatus. United States patent US 2014/0067283 A1, 2014 Mar. 6. Available at: https://patents.google.com/patent/US20140067283A1/en.

The authors declare that there are no conflicts of interest present.