Method for detecting content of oxytetracycline hydrochloride
A technology of oxytetracycline hydrochloride and detection method, which can be applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as impurity and complicated operation, and achieve the effects of high recovery rate, simple operation, good stability and repeatability
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Embodiment 1
[0043] Embodiment 1: use the method for high-performance liquid chromatography detection oxytetracycline hydrochloride content
[0044] Take 100mL of purified water, add 5.23g of dipotassium hydrogen phosphate, dissolve and add sodium hydroxide to adjust the pH to 8.0.
[0045] Take 400mL of purified water, add 120g of tert-butanol, after dissolving, add 100ml of the above-mentioned dipotassium hydrogen phosphate solution, mix well, and filter to obtain the mobile phase;
[0046] Take 1000mL of purified water, add 4.5mL of concentrated hydrochloric acid, mix well, and prepare a diluted solution;
[0047] Take about 44mg of oxytetracycline hydrochloride, accurately weigh it, put it in a 100ml measuring bottle, add 0.05mol / L hydrochloric acid solution to dissolve and dilute to the mark, shake well, accurately measure 5ml, put it in a 10ml measuring bottle, add 0.05mol / L The hydrochloric acid solution is diluted to the mark, shakes up, makes need testing solution;
[0048] Take...
Embodiment 2
[0051] Embodiment 2: Dipotassium hydrogen phosphate solution and tert-butanol ratio investigation
[0052]Three mobile phases with volume ratios of 10:90, 20:80, and 30:70 were prepared by using the solution containing 0.3 mol / L dipotassium hydrogen phosphate and tert-butanol prepared according to Example 1. The rest of the conditions are the same as in Example 1, and the resolution, main peak retention time and impurity peak quantity of different mobile phases are shown in Table 1.
[0053] Table 1 The resolution, main peak retention time and impurity peak quantity of different mobile phase ratios
[0054]
[0055] It can be seen that, with the reduction of tert-butanol in the mobile phase, the retention time of the main peak is prolonged, and the separation degree of the main peak and adjacent impurities is the best when the ratio of dipotassium hydrogen phosphate solution and tert-butanol is 20:80 Good, and the retention time of the main peak is moderate compared to the...
Embodiment 3
[0056] Embodiment 3: the investigation to dipotassium hydrogen phosphate solution concentration
[0057] Take 100mL of purified water, add 0.1mol (1.74g), 0.2mol (3.48g), 0.3mol (5.23g) and 0.4mol (6.97g) of dipotassium hydrogen phosphate, dissolve and add sodium hydroxide to adjust the pH to 8.0, take 100ml of the above solution was mixed with 400ml of tert-butanol solution (concentration: 0.3g / mL), filtered, and four mobile phases were prepared respectively. All the other conditions are the same as in Example 1. The resolution, retention time of main peak and number of impurity peaks of different mobile phases are shown in Table 2.
[0058] Table 2 The degree of separation and the retention time of the main peak and the number of impurity peaks of different concentrations of dipotassium hydrogen phosphate solution
[0059]
[0060]
[0061] As the concentration of dipotassium hydrogen phosphate increases, the retention time of the main peak is relatively advanced, an...
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