Determination of Azithromycin Tablets
【Abstract】 Objective: To establish a rapid and accurate UV spectrophotometric determination of azithromycin tablets. Methods: The reference to azithromycin tablets dissolution rate determination method using ethanol and 0.1 mol / L hydrochloric acid as solvent, 75 ? 100 sulfuric acid solution
as the chromogenic agent, at room temperature, color 30 min, and then measured at 482 nm wavelength significantly After the solution color absorption, and after color calculated by
comparing the standard solution of azithromycin in tablets, and compared with the micro-determination method. Results:
Azithromycin in the 7.5 ~ 52.5 μg / mL concentration range of
absorbance A and concentration C into a linear correlation
between the regression equation A = 0.0201C-0.1059, r =
0.9999; recovery (99.7 ? 0.31) %, RSD = 0.3%, the sample
measurement results and microbiological processes are consistent. Conclusion: The method is simple, accurate and suitable for control of azithromycin tablets.
Key words azithromycin; spectrophotometry; content; determination
Azithromycin (Azithromycin) is 15-membered ring macrolide
antibiotics, erythromycin antibacterial spectrum and are similar to the Streptococcus pyogenes, Streptococcus
pneumoniae and Haemophilus influenzae are bactericidal effect on the part of the Staphylococcus with a stunning bacteria, mainly used in clinical respiratory tract, skin and soft tissue infections and Chlamydia trachomatis urethritis and cervicitis caused by infectious diseases such as . Azithromycin tablet common dosage forms, 2005 edition of "Chinese Pharmacopoeia" content detection method is microbiological method . This method is cumbersome,
inspection cycle is long, many factors, not suitable for rapid
analysis of samples. In addition, the chemical structure of azithromycin on non-conjugated double bonds, no characteristic absorption in the UV region can not be the direct use of UV spectrophotometry determination of its quality. I refer to the
dissolution of azithromycin tablets determination , and refer to the same drug Determination of roxithromycin capsule , was established by spectrophotometry rapid detection method of Azithromycin Tablets are the results reported are as follows.
An instrument and reagent
760CRT UV-Vis spectrophotometer (Shanghai Precision Scientific Instrument Co., Ltd.); fine days FA2004A analytical balance (Shanghai Ryohei Instrument Co., Ltd.).
Azithromycin raw materials (content 95.3%, batch number: 20,060,607) to Zhengzhou Yonghe Pharmaceutical Co., Ltd. as gifts, Azithromycin reference substance (952 u / mg) were purchased from China Pharmaceutical and Biological Products Institution, Azithromycin Tablets (Henan Fu Jen Tang
Pharmaceutical Co., Ltd., batch number:
20060703,20060905,20061014) were purchased from pharmacies, other reagents were analytical pure.
2 Methods and Results
2.1 Preparation of Solution
2.1.1 Preparation of reference substance reserve liquid
Precision Weigh 105 ? drying to constant weight of
azithromycin reference substance 75.0 mg, placed in 100 mL flask, add the appropriate amount of ethanol (each 2 mg of azithromycin plus ethanol 1 mL) dissolved and add 0.1 mol / L
hydrochloric acid constant volume, as a reserve liquid.
2.1.2 Preparation of reference substance solution
Precise amount of the reserve fluid 16.7 mL take place 25 mL flask, add 0.1 mol / L hydrochloric acid and is scheduled
to allow adequate shaking, as a reference substance solution.
2.1.3 Solution preparation for the test items
To take this product 10, that setting precision and research small, sophisticated take that amount of powder (approximately equivalent to azithromycin 25.0 mg) placed in 50 mL flask, add the appropriate amount of ethanol (each 2 mg of azithromycin plus ethanol, 1 mL) dissolved, then add 0.1 mol / L hydrochloric acid shake and is scheduled to capacity. Filtering, abandoned to the beginning of the filtrate, take
continued filtrate as a solution for the test items.
2.1.4 Blank solution preparation accessories
In accordance with the proportion of preparation does not contain the main prescription drug gap accessories, in accordance with "2.1.3" for test preparation materials solution method of preparation of a blank solution accessories.
Precise amount of test items taken for the reference substance and the solution of 5 mL were placed in 50 mL flask,
add 0.1 mol / L hydrochloric acid shake and is scheduled to capacity, made for every 1 mL containing 50 μg of
azithromycin solution. Precise amount again to take the solution of 5 mL were placed in 10 mL flask, add sulfuric acid solution (75 ? 100) 5 mL shake, put it aside at room
temperature for 30 min.
After taking the above-mentioned color solution to 0.1
mol / L hydrochloric acid as a blank, according to spectrophotometry (Appendix ? A) , in the wavelength of
482 nm absorbance was measured to calculate the content of
azithromycin. Reposted elsewhere in the paper for free download http://
2.3 Determination of Wavelength Selection
Take "2.2" under the color of the reference substance
after the solution to 0.1 mol / L hydrochloric acid as blank,
in the 400 ~ 550 nm wavelength range scans. Azithromycin in the 482 nm wavelength at maximum absorption. At the same time taking "2.1.4" blank excipients solution with the method is drug-free absorption characteristic wavelengths accessories,
does not affect the determination of azithromycin. Therefore, in accordance with its wavelength characteristics, chosen as a measurement wavelength of 482 nm, UV-scanning pattern shown in
2.4 The standard curve drawing
Precise amount of each check, "2.1.1" reference substance placed in reserve liquid 1.0,2.0,3.0,4.0,5.0,6.0,7.0 mL in 50 mL flask, add 0.1 mol / L hydrochloric acid constant volume to the scale, made of each ml, respectively
15.0,30.0,45.0,60.0,75.0,90.0,105.0 μg azithromycin solution;
precise amount of each check and then 5 mL of the solution placed in 10 mL flask, add sulfuric acid solution (75 ? 100 )
5 mL, shake, made with azithromycin, respectively 7.5,15.0,22.5,30.0,37.5,45.0,52.5 μg of the solution, put it
aside for 30 min. With 0.1 mol / L hydrochloric acid as blank, in the wavelength of 482 nm absorbance was measured, and to absorb the degree of concentration of C the corresponding A linear regression was the regression equation. Azithromycin in the 7.5 ~ 52.5 μg / mL concentration range, regression
equation was A = 0.0201C-0.1059, r = 0.9999, n = 7, a linear
relationship was good.
2.5 Solution stability test
Take "2.4" under the series of concentrations of azithromycin color solution, placed in a water bath at 37 ?,
respectively, 15.0 min, 30.0 min, 1.0 h, 1.5 h, 2.0 h sampling, the wavelength of 482 nm in the repeated measurements, The results at 37 ? water bath to place 2.0 h,
solution absorbance changes of less than 1.0%; in the samples at room temperature in 30.0 min, 1.0 h, 1.5 h, 2.0 h, 4.0 h sample absorbance measurement, the solution absorbance changes of less than 1.0 %.
2.6 recovery test
Precision said fixed amount of azithromycin reference
substance, according to method of azithromycin tablets made of
high, medium and low concentrations of azithromycin tablets analog tablets, and then follow the "2.1" method under the the preparation of solution and the "2.2" under the method of determination, each sample measured two times, taking the
average to calculate the recovery rate, the results in Table 1.
Table 1 Determination of Azithromycin recovery test results (omitted)
2.7 Precision tests
To take the tablets prepared in accordance with "2.1" solution, under the method of preparation, the concentration of five samples of each, and then follow the "2.2" were measured under the concentration. Continuous determination of 5 d, the calculation precision day and day. The results of days of RSD = 0.7%, during the day RSD = 1.8%, showed a
smaller variation between the determination results, methods, good precision.
2.8 Determination of Sample
Sanpi azithromycin tablets taken in accordance with "2.2" under the method for the determination and the 2005 edition of
"Chinese Pharmacopoeia" potency micro-organisms were measured
to calculate the amount of labeled samples to compare the results of the two measurement methods consistent sex. The results of three batches of samples labeled azithromycin volume at 98.0% ~ 103.0% range meet the pharmacopoeia
requirements, specific results in Table 2. Table 2 Sample assay results (omitted)
Determination of Azithromycin Tablets Azithromycin content and the use of micro-organisms Pharmacopoeia potency
determination of the results more consistent, but the spectrophotometric method is more simple, rapid, accurate and more suitable for the production sector of the intermediate control and health supervision departments of the rapid test analysis.
Color with sulfuric acid, the sulfuric acid dosage, concentration and temperature affect the reaction results, this reference to azithromycin tablets dissolution testing methods for the selection of 75 ? 100 of the sulfuric acid
solution, color, and make the temperature of a balanced
solution to the at room temperature after the determination of the maximum response reduced the difference between the finished solution, helps to maintain the consistency of the results.
Sulfuric acid color reaction, can emit a lot of heat, so
in order to maintain consistency between samples need to be aware of sulfuric acid by adding the speed should be relatively slow, so that heat can be evenly distributed gradually go out with each other as consistent as possible.
 JIANG Ming-Xing. New Practical pharmacology [M]. 2nd edition. Beijing: Science Press, 2005: 622 624.
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 HE Li-Ming, Zhang Hui-Wen, Zeng Xiao-hui. Ultraviolet
Spectrophotometry Determination of Roxithromycin Capsules [J]. Guangdong College of Pharmacy, 2004, 20 (5): 475 477.
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Republic of China Pharmacopoeia (2) [S]. Beijing: Chemical Industry Press, 2005: Appendix ? A 22 23. Reposted
elsewhere in the paper for free download http://