Development of a Procedure for the Identification of Pharmaceutical Substance «Buserelin Acetate» by NMR Spectroscopy without Using Pharmacopoeia Reference Standard
Abstract
The identification of the buserelin acetate sample was carried out without using the pharmacopeia reference standard. The identification was based on the spectral NMR data (1H,13C,1H-1H gCOSY,1H-13C gHSQC,1H-13C gHMBC) complex analysis. NMR experiment parameters were determined for the obtaining of spectra with S/N ratio above 50: 1 (1H) and 10:1 (13C). The inexpediency of using the acetate anion signal for calibration of the scale of chemical shifts in the spectra of an aqueous solution of buserelin acetate is shown. The assumption about the effect of the speed of prototropic tautomerism on the disappearance of signals of carbon atoms in positions 4 and 5 of the imidazole ring in the L-histidine fragment of buserelin acetate was made.
About the Authors
N. E. Kuzmina
Scientific centre for expert evaluation of medical products of the Ministry of Health of Russian Federation
Russian Federation
Russian Federation
S. V. Moiseev
Scientific centre for expert evaluation of medical products of the Ministry of Health of Russian Federation
Russian Federation
Russian Federation
V. I. Krylov
Scientific centre for expert evaluation of medical products of the Ministry of Health of Russian Federation
Russian Federation
Russian Federation
V. A. Yashkir
Scientific centre for expert evaluation of medical products of the Ministry of Health of Russian Federation
Russian Federation
Russian Federation
V. A. Merkulov
Scientific centre for expert evaluation of medical products of the Ministry of Health of Russian Federation
Russian Federation
Russian Federation
References
1. Mezo I., Lovac S., Palyi I., Vincze B., Kalnay A., Turi G. et al. Synthesis of Gonadotropin-Releasing Hormone III Analogs. Structure-Antitumor Activity Relationships. J Med Chem 1997; 40 (21): 3353-3358.
2. Хасханова Л.Х., Пиддубный М.И., Ордиянц И.М., Плаксина Н.Д., Погасов А.Г., Золичев Г.Е. и др. Вестник РУДН, сер. Медицина. Акушерство и гинекология 2002; 1: 225-227.
3. Сафронова Е.Ю., Крашенинников А.А., Сергиенко С.А., Костин А.А. Использование современных аналогов лютеинизирующего гормона рилизинг-гормона при проведении гормональной терапии у больных раком предстательной железы. Исследования и практика в медицине2017; 4 (2): 23-28
4. Monograph 01/2017:1077 Buserelin. in: European Pharmacopoeia, 9th ed. V.1. Strasbourg: European Department for the Quality of Medicines & Health Care; 2016. p. 1887-1889.
5. General monograph 5.12 Reference standards. in: European Pharmacopoeia, 9th ed. V.1. Strasbourg: European Department for the Quality of Medicines & Health Care; 2016. p. 733-738.
6. Кузьмина H.E., Моисеев C.B., Яшкир В.А., Осинцева Е.В. Возможности использования метода ядерного магнитного резонанса при аттестации стандартных образцов. Стандартные образцы 2014; 2: 19-25.
7. Лутцева А.И., Боковикова Т.Н., Яшкир В.А., Стронова Л.А., Кузьмина Н.Е., Агапкина М.В. и др. Методологические подходы к выбору методов установления подлинности лекарственных средств. Ведомости НЦ ЭСМП 2017; 7 (2): 71-76
8. General monograph 2.2.64 Peptide identification by nuclear magnetic resonace. in: European Pharmacopoeia, 9th ed. V.1. Strasbourg: European Department for the Quality of Medicines & Health Care; 2016; 112
9. ФС.1.1.0012.15 Валидация аналитических методик в ГФ РФ, XIII изд. Т. 1. Москва: Изд-во Министерства здравоохранения РФ; 2015; 222-234.
10. Кузьмина Н.Е., Моисеев С.В., Крылов В.И., Яшкир В.А., Меркулов В.А. Возможности метода ЯМР спектроскопии при определении микрокомпонентов смесей. Журнал аналитической химии 2014: 69 (11): 1152-1160.
11. Gottlieb H.E., Kotlyar V., Nudelman A. NMR chemical shifts ofcommon laboratory solvents as trace impurities. J Org Chem 1997; 62 (21): 7512-7515.
12. Ларина Л.И. Спектроскопия ЯМР и строение замещенных азолов. Автореферат дис. док. хим. наук. Иркутск: Иркутский гос. унив. 2003.
Review
For citations:
Kuzmina N.E., Moiseev S.V., Krylov V.I., Yashkir V.A., Merkulov V.A. Development of a Procedure for the Identification of Pharmaceutical Substance «Buserelin Acetate» by NMR Spectroscopy without Using Pharmacopoeia Reference Standard. Antibiot Khimioter = Antibiotics and Chemotherapy. 2017;62(9-10):40-46. (In Russ.)
Views:
380
Email this article 