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The objective of this work was developed for the quantification of doxycycline and tetracycline in pharmaceutical products for proposed protocol describes the use of iron ion contained in vitamin tablets as reagent. It is based on the complexation between drugs - iron ion in acidic and dilution of hydrogen peroxide. Method: This study was used commercial doxycycline and tetracycline in samples for capsules and tablets which was reacted with iron ion from vitamin tablets was concentration 5.0 ´ 10-2 mol/L in 5.0 ´ 10-3 mol/L nitric acid and 2.5 ´ 10-2 % (v/v) of hydrogen peroxide as reagent in a ratio of 2.0 : 1.0 : 0.1 (v/v), respectively. The reaction was given a yellow complex with the optimum absorption at 425 nm. Results: The calibration graphs were contained doxycycline and tetracycline standard in the range of 1.0 - 100 mg/mL and 1.0 - 200 mg/mL, respectively. Linear regression analysis of the absorbance of each drug (y) and concentration of each drug (x) expressed the equation y = 0.0064x – 0.001 (r2 = 0.9998) and y = 0.0069x - 0.0095 (r2 = 0.9997) for doxycycline and tetracycline, respectively. The limit of detection (LOD) and limit of quantitation (LOQ) each drug was 1.2, 4.0 mg/mL and 0.1, 0.4 mg/mL for doxycycline and tetracycline, respectively. The percentage relative standard deviation (RSD) of the repeatability for this proposed method was less than 2.00 %, the percentage recovery was in the range 98.62 - 100.56 % for doxycycline and 100.92 - 102.00 % for tetracycline. Conclusion: This proposed method was successfully applied in the determination of doxycycline and tetracycline in pharmaceutical products. The results obtained by the proposed method were in good agreement with method by the student t-test at the 95% confidence level.
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