STABILITY-INDICATING HPLC METHODS FOR DRUG ANALISYS
edited by Quanyun A. Xu
Editorial: Pharmaceutical Press & American
Pharmacists Association (APha)
Páginas:
912
Año: 2008
Edición:
3era Edición
Presentación:
Encuadernado
País
de Procedencia: Inglaterra
Publicación
Técnica y Científica para los profesionales en el campo de la ciencia
farmacéutica en general. los analistas que participan en la evaluación de la
estabilidad del fármaco, departamento de desarrollo, Control de Calidad,
Regulación de Medicamentos, Académicos y profesionales relacionados al sector
farmacéutico.
Stability-Indicating HPLC Methods for Drug Analysis,
third edition, is structured a series of monographs on 572 different drug
entities, including 96 new in this edition. These monographs have been prepared
from 851 published references and present 1,028 stability-indicating HPLC
analytical methods. The information that is presented in the monographs has
been gathered from the published literature and is summarized in a structured
textual format composed of 30 elements.
In depth description of the HPLC analysis presented in
original publication.
Components
The first series of monograph elements were obtained
from standard reference works. This information in the basic information
analyst may find useful in analyzing various drug products. The information
presented includes:
1. Chemical name (s)
2. Molecular structure
3. Other name (s)
4. Form (s) of the drug molecule available in drug
products
5. Molecular formula
6. Molecular weight
7. CAS number
8. Appearance and description
9. solubility’s
10. pKa values
The
Basic information in followed by one or more summaries of previously published
stability – indicating analytical, methods. The summaries follow a highly
structured ext format. Each of the informational items that follow is included
when presented in the original published articles.
The
reader should recognize that all too often one or more pieces of information
were omitted in the original work and, consequently, do not appear in this compilation.
However, the summaries have been made as complete as possible from the original
published articles.
The first section of the method summary includes the
following information:
11. Individual (s) who developed or published the
method
12. Drug, salt form (if applicable), and presentation
that was analyzed
13. Description of analytical system components
14. Description of column
15. Mobile phase composition and flow rate
16. Detection wavelength and sensitivity
17. Internal standard (if present)
The second section of the method includes:
18. Standard solution preparation
19. Sample preparation (dilution, extraction,
derivatization, etc.)
20. Injection volume
21. Retention times for subject drug, secondary drug
(s), and internal standard
The third section of the summary describes the
demonstration of the Stability indicating nature of the method. The description
includes:
22. The decomposition techniques and/or sample spiking
that was used
23. Absence of interference of decomposition product
with intact drug
24. Retention times for intact drug and degradation
product.
The fourth section of the method summary includes the
following Information:
25. Concentration range of the standard curve
26. Correlation coefficient and linearity
27. Coefficient of variation of the assay
28. Intraday and intraday coefficients of variation of
the samples
29. Limit of detection and limit of quantitation.
And lastly, the source of the method is presented:
30. Reference (s)
The reference (s) form the published literature that
utilized the particular method provides proper attribution and allows readers
to more easily refer to the original work if that would be useful.
It has always seemed to us that the best starting
point in identifying a suitable stability-indicating analytical method is from
methods that have previously been shown to be stability indicating in studies
by other researchers. Of course, finding an analytical method in the literature
that has been found to be stability indicating in a previous study does not
preclude the need to evaluate the methods in the analyst’s hands. The analyst
is still obligated to assure the adequacy of the methods for specificity,
precision, reproducibility, and sensitivity. Furthermore, the methods must be
shown to separate and quantify the intact drug in the presence of its
decomposition products and other dosage form components. However, this task of
finding a suitable methods and documenting that it is both stability indicating
and is functioning properly in one’s own laboratory is aided when the analyst
start with a methods that has been shown by other to be stability indicating.
Analysis must also be aware that the presentation of a
stability-indicating analytical method in the literature does not absolve them
of the method in their own laboratory. The analysis still must determine
fundamental performance parameters of the method including sensitivity,
precision, reproducibility, and accuracy. Also, the stability-indicating ability
of the analyst’s laboratory to demonstrate that the method is working properly.
These are more likely to be easily achievable when the method has been shown to
work in another analyst’s hands.
