Romero DJA, Begue DM, Gato MA

Language: Spanish
References: 8
Page: 436-445
PDF size: 137.77 Kb.

ABSTRACT

Objective: to develop and validate an analytical high-performance liquid chromatography method applicable to quality control and to stability study of 2 % Dorzolamide plus 0.5 % Timolol eye drops.
Methods: to simultaneously quantify both active principles in the finished product, separation was made through a Luna RP-18 (5 µm) (250 x 4 mm) column chromatography, with photodiode array detector at 254 nm an 295nm using a gradient with mobile phase A composed of acetonitrile: phosphate buffer pH 2.5: methanol (5:85:10) and mobile phase B: methanol and the quantification of this front to a reference sample using the external standard method.
Results: in the linearity study, the correlation and determination coefficients were above 0.99 and 0.98 respectively. The percentages of having recovered were 99.57 for Dorzolamide and 99.93 for Timolol, with a variation coefficient for both active principles under 2 %. In the repeatability study, the means were 99.1 for Dorzolamide and 100.4 % for Timolol and the variation coefficients were within the set limits. In the study of intermediate precision, p values were higher than 0.05 for each of the studied levels.
Conclusions: the developed analytical method was linear, precise, specific and accurate in the range of study concentrations; it is established for the quality control and stability study of the finished product since there were not analytical methods designed for these aims.

REFERENCES

1. Toris CB, Zhan GL, Yablonski ME. Effects on aqueous flow of dorzolamide combined with either timolol or acetazolamide. lamide. J Glaucoma. 2004;13 (3):210-5.

2. Kiland JA, Gabelt BT, Kaufman PL. Studies on the mechanism of action of timolol and on the effects of suppression and redirection of aqueous flow on outflow facility. Exp Eye Res. 2004;78(3):639-51.

3. Farmacopea de los Estados Unidos. USP 34. The United States Pharmacopeial Convention. Versión electrónica. New York: Pharm Convention; 2011.

4. Dierksneier G. Métodos cromatograficos. La Habana: Ed. Científico-Técnica; 2005. p. 1-4, 256-412.

5. Guidance for Industry. Analytical Procedures and Methods Validation Chemistry, Manufacturing, and Controls Documentation. New York: FDA/Center For Drug Evaluation and Research; 2001.

6. International Conference on Harmonization. Validation of Analytical Procedures. Technical Requirements for the Registration of Pharmaceuticals For Human Use. Geneva: ICH-Q2A; 1995.

7. Farmacopea de los Estados Unidos. USP 30. The United States Pharmacopeial Convention. Versión electrónica. New York: Pharm Convention; 2007.

8. Colectivo de autores. Analytical Profiles of Drug Substances. vol 16. New Jersey: Klaus Florey,1987.