Hernández FD, Ledea LOE, Fernández GLA, González GE

Language: Spanish
References: 15
Page: 219-231
PDF size: 251.04 Kb.

ABSTRACT

Introduction: caffeine is a substance located in some plants like coffee, tea, cocoa; it is also an ingredient of some drugs such as analgesics, a metabolic and central nervous system stimulant. The consumption of caffeine either acute or chronic may give rise to a variety of adverse effects. Due to its use in the drug industry, it is vitally important to determine it. The validation of an analytical method scientifically proves that it is adequate for a particular application as in the case of determination of active ingredients in aqueous solutions.
Objective: to validate an analytical method for the quantitation by means of high performance liquid chromatography of the caffeine content in aqueous solutions and in wastewater samples from a drug manufacturing laboratory.
Methods: the validation of the chromatographic method was performed by using a RP—18 de 250 x 4,6 mm, 5 µm column, a mobile phase: water/ CH₃OH (70/30); Flow: 1,0 mL/min and an ultraviolet detector at 254 nm. The caffeine content was estimated by the high performance liquid chromatograpy following the international regulations in force.
Results: the method was selective against the ozonization products, linear r = 0.999 y r² = 0.999), precise, accurate, robust and sensitive in the 1x10^-4mol/L to 2x10^-3mol/L interval. The analyte stability was also evaluated under the analysis conditions. The caffeine content in wastewaters of the drug manufacturing industry was determined at concentrations lower than 3x10^-4 mol/L.
Conclusions: the validated method was selective, linear, precise, accurate and robust in the analyzed interval of concentrations and allows estimating the caffeine content in aqueous solutions and of the analyte in wastewater samples from a pharmaceutical laboratory that produces the drug in Cuba.

REFERENCES

1. International Food Information Council Foundation. Caffeine & Health: Clarifying the controversies. IFIC Review 2008. [Citado: 4 de enero de 2014]. Disponible en: http://www.ific.org

2. Kari R, Virpi R, Jouko L, Pertti N. Effect of Caffeine- Containing versus Decaffeinated Coffee on Serum Clozapine Concentrations in Hospitalised Patients Basic. Clin Pharmacol Toxicol. 2004;94:13-8.

3. Brown GK, Zaugg SD, Barber LB. Wastewater analysis by gas chromatography / mass spectrometry. Water Resources Investigations. Rep. U.S. Geol Surv. 1999;99 4018B:431-5.

4. Wanyika HN, Gatebe EG, Gitu LM, Ngumba EK, Maritim CW. Determination of caffeine content of tea and instant coffee brands found in the Kenyan market. African Journal of Food Science. 2010;4(6):353-358.

5. Komes D, Horžić D, Belščak A, Kova K and Baljak A. Determination of Caffeine Content in Tea and Maté Tea by using Different Methods. Czech J. Food Sci. Special Issue. 2009;27.

6. Švorc Ľ. Determination of Caffeine: A Comprehensive Review on Electrochemical Methods. Int. J. Electrochem. Sci., 2013;8:5755-73.

7. Weimann A, Sabroe M, Poulsen HE. Measurement of caffeine and five of the major metabolites in urine by high-performance liquid chromatography/tandem mass spectrometry. J. Mass Spectrom. 2005;40:307-316.

8. Patil, Pandurang N. Caffeine in various samples and their analysis with HPLC - A review. International Journal of Pharmaceutical Sciences Review & Resear. 2012;16(2):76.

9. Anand patil, varun raheja, anagha cafeínamre. Simultaneous analysis of intestinal permeability markers, caffeine, paracetamol and sulfasalazine by reverse phase liquid chromatography: a tool for the stancafeínardization of rat everted gut sac model. Asian Journal of Pharmaceutical and Clinical Research. 2010;3(3):204-7.

10. EURACHEM Guide: The Fitness for Purpose of Analytical Methods. A Laboratory Guide to Method Validation and Related Topics. First English Edition 1.0; 1998.

11. U.S. Food and Drug Administration. FDA Technical Review Guide; Center for Drug Evaluation and Research (CDER), Guidance for Industry, Analytical Procedures and Methods Validation, Chemistry Manufacturing and Controls Documentation, Draft Guidance; 2000. [Citado: 4 de enero de 2014]. http://www.fda.gov/downloads/Drugs/GuidanceComplianceRegulatoryInformation/ Guidance/ucm122858.pdf

12. The United States Pharmacopoeia. United States Pharmacopoeial Convention: Rockville, Md; 2009.

13. ICH –Harmonised tripartite Guideline. Validation of analytical Procedures: Text and Methodology Q2 (R1); 2005.

14. WHO- Technical Report Series No. 937. Appendix 4n Analytical Method Validation; 2006.

15. Bonfilio R, Laignier EC, Benjamim M, Nunes HR. Analytical Validation of Quantitative High-Performance Liquid Chromatographic Methods in Pharmaceutical. Analysis: A Practical Approach, Critical Reviews in Analytical Chemistry. 2012;42(1):87-100.