System Suitability Requirements for Liquid Chromatography Methods: Controlled Parameters and their Recommended Values (Review)
Tóm tắt
Chromatographic analytical results can be affected by various factors associated with the chromatographic system. Requirements for system suitability testing (SST) are introduced to minimize the risk of such factors having a critical influence on the results. This review covers the chromatographic parameters for SST and their recommended values and categorizes them into five groups depending on the purpose for their introduction into the SS requirements. The type of method (isocratic or gradient) and purpose of the testing (determination of the main substance or impurity content, peak asymmetry, etc.) are considered. Some additional intralaboratory parameters for SST in serial analyses (routine testing) are studied. Arecommendation to introduce the condition N ≥ 0.9Nexp, where Nexp is the smallest experimental number of theoretical plates N at which the requirements for system sensitivity (S/N, signal/noise) is still fulfilled for testing before and during the method validation, is given for the first time for gradient methods of impurity determination. This condition is justified from a theoretical viewpoint. Attention is drawn to the expediency of robustness testing to refine the SST requirements. Information given in this review supplements significantly recommendations of the European Pharmacopoeia, US Pharmacopeia, and the State Pharmacopoeia of the Russian Federation for chromatographic SST. These recommendations are important for improving the reliability of chromatographic system suitability control.
Tài liệu tham khảo
United States Pharmacopoeia, Chromatography, USP40-NF35 (2017).
European Pharmacopoeia, 9.5th Ed., Chap. 2.2.46, Chromatographic Separation Techniques, EDQM, Strasbourg (2018).
State Pharmacopoeia of the Russian Federation, XIVth Ed., Vol. 1, Moscow (2018), pp. 862 – 865.
ICH Harmonised Tripartite Guideline, Validation of Analytical Procedures: Text and Methodology Q2(R1), ICH (2005); 13. https: //database.ich.org/sites/default/files/Q2_R1_Guideline.pdf.
N. A. Epshtein and S. V. Emshanova, Khim-farm. Zh., 42(11), 34 – 40 (2008).
V. V. Beregovykh (ed.), Validation of Analytical Methods for Drug Manufacturers. Typical Guideline for Drug Manufacturing Plants [in Russian], Litterra, Moscow (2008).
J. Ermer and J. H. McB. Miller (eds.), Method Validation in Pharmaceutical Analysis: A Guide to Best Practice, Wiley- VCH, Weinheim, 2005.
N. A. Epshtein, V. L. Sevast’yanova, and A. N. Koroleva, Razrab. Regist. Lek. Sredstv, 7(1), 96 – 110 (2018); https: //www.pharmjournal.ru/jour/article/view/552/0; N. A. Epshtein, V. L. Sevastianova, and A. I. Koroleva, URL: https: //www.researchgate.net/publication/323801207_INVESTIGATIONo._OF ROBUSTNESS_AT_VALIDATIONo._OF HPLC_ AND_UPLC_METHODS_A_MODERNo._APPROACH INCLUDING_ RISK_ANALYSIS/stats).
J. C. Wahlich and G. P. Carr, J. Pharm. Biomed. Anal., 8(8 – 12), 619 – 623 (1990); https: //www.sciencedirect.com/science/article/abs/pii/0731-7085(90)8009-13.
Reviewer Guidance: Validation of Chromatographic Methods, Center for Drug Evaluation and Research (CDER). Washington (1994); https: //www.fda.gov/downloads/drugs/guidances/ucm134409.pdf.
Technical Guide for the Elaboration of Monographs, 7th Ed., EDQM, European Pharmacopoeia (2015), pp. 30 – 32; https: //www.edqm.eu/sites/default/files/technical_guide_for_the_elaboration_of_monographs_7th_edition_2015.pdf.
K. Sychev, Analitika, 2(3), 60 – 66 (2012); http: //www.j-analytics.ru/files/article pdf/3/article 3204 700.pdf.
P. C. Sadek, Troubleshooting HPLC Systems. A Bench Manual, John Wiley & Sons, Inc., New York (2000) [Russian transl., I. Dubinskii, Moscow (2010)].
L. R. Snyder, J. J. Kirkland, and J. L. Glajch, Introduction to Modern Liquid Chromatography, 3rd Ed., JohnWiley and Sons, Hoboken, New Jersey (2010).
S. W. Baertschi, K. M. Alsante, and R. A. Reed (eds.), Pharmaceutical Stress Testing: Predicting Drug Degradation, 2nd Ed., Informa Healthcare, New York (2011).
N. A. Epshtein, Razrab. Regist. Lek. Sredstv, 3(16), 118 – 132 (2018); https: // www.pharmjournal.ru/jour/article/view/298/294.
N. A. Epshtein, Razrab. Regist. Lek. Sredstv, 3(24), 116 – 128 (2018); https: // www.pharmjournal.ru/jour/article/view/612.
D. R. Jenke, J. Liq. Chromatogr. Relat. Technol., 19(12), 1873 – 1891 (1996); https://doi.org/10.1080/10826079608014012.
Y. Vander Heyden, M. Jimidar, E. Hund, et al., J. Chromatography A, 845, 145 – 154 (1999); https: //www.sciencedirect.com/science/article/pii/S0021967399003283.
Y. Vander Heyden, A. Nijhuis, J. Smeyers-Verbeke, et al., J. Pharm. Biomed. Anal., 24(5 – 6), 723 – 753 (2001); https://www.sciencedirect.com/science/article/abs/pii/S073170850000529X.
E. Hund, Y. Vander Heyden, D. L. Massart, and J. Smeyers-Verbeke, J. Pharm. Biomed. Anal., 30, 1197 – 1206 (2002); https: //www.sciencedirect.com/science/article/abs/pii/S0731708502004703.
P. K. Sahu, J. Anal. Bioanal. Tech., 8(3), 1 – 8 (2017); https://doi.org/10.4172/2155-9872.1000363.
N. A. Epshtein, Khim.-farm. Zh., 38(3), 40 – 56 (2004).
J. W. Dolan, “Column Plate Number and System Suitability,” LCGC North America, 34(3), pp. 190 – 197 (2016); http: //www.lcresources.com/tsbible/34032016.pdf.
N. A. Epshtein, Razrab. Regist. Lek. Sredstv, 8(1), 108 – 112 (2019); doi: https://doi.org/10.33380/2305-2066-2019-8-1-108-112.
N. A. Epshtein, Vedom. NTsESMP, 7(2), 85 – 91 (2017); https://www.vedomostincesmp.ru/jour/article/view/124/123.
N. A. Epshtein, V. L. Sevast’yanova, and A. I. Koroleva, Razrab. Regist. Lek. Sredstv, 3(24), 182 – 188 (2018).
N. A. Epshtein, Khim.-farm. Zh., 53, No. 12, 48 – 57 (2019); doi: https://doi.org/10.30906/0023-1134-2019-53-12-48-57.
Questions and Answers on Current Good Manufacturing Practices – Laboratory Controls, U. S. Food and Drug Administration; https: //www.fda.gov/drugs/guidances-drugs/questionsand-answers-current-good-manufacturing-practices-records-and-reports.