Separation method and application of related impurities of timolol compound and timolol maleate
A technology of timolol maleate and related impurities, which is applied in the separation of timolol compounds and related impurities of timolol maleate and its application field, can solve the problem of high performance liquid chromatograph damage and difficult impurities. Solve problems such as separation and solvent volatility, and achieve the effect of strong specificity, high sensitivity, and simple operation
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Embodiment 1
[0056] 1. Instrument: Shimadzu LC-20AT, the detector model is SPD-M20A electronic analytical balance of Sartorius Scientific Instrument Co., Ltd., model is SECURA125.
[0057] 2. High performance liquid chromatography conditions:
[0058] Mobile phase: methanol: acetonitrile = 10:90 (add 50mmol formic acid and 25mmol diethylamine to the mixed solution, accounting for 0.45% of the mobile phase volume)
[0059] Chromatographic column ZWIX(+)150×4mm, 4.0μm;
[0060] The detection wavelength is 298nm;
[0061] The column temperature is 25°C;
[0062] Flow rate 0.5ml / min.
[0063] 3. Measurement method:
[0064] 3.1 Accurately weigh the appropriate amount of S-timolol (manufacturer: EP, batch number: Batch3.0) and R-timolol (manufacturer: EP, batch number: Batch3.0) reference substance, add methanol to dissolve and dilute to each A solution containing 1 mg of S-timolol and 0.1 mg of R-timolol in 1 ml was used as a systemic suitability solution.
[0065] Experiments were car...
Embodiment 2
[0081] Carry out the experiment with reference to the sample and operating method of 3.1 of Example 1, the difference is that the mobile phase is methanol: acetonitrile=15:85 (add 50mmol formic acid and 25mmol diethylamine to the mixed solution, the percentage of the amount added is 0.45%) . Obtain efficient chromatogram, the result is as follows:
[0082]
[0083] Among them, peak number 1 is maleic acid; peak number 2 is R-timolol; peak number 3 is S-timolol.
[0084] The results show that the chromatographic conditions can effectively separate S-timolol, R-timolol and maleic acid, and the peak shape is better, the baseline is more stable, and the resolution is greater than 1.5.
[0085] 3.4 Sample recovery experiment
[0086] Accuracy is obtained by adding 80%, 100% and 120% of the recovery rate of three different concentrations of R-timolol stock solution (2μg / ml) in the test solution, adding a known amount of R-timolol Lol, then measure the ratio (recovery rate) bet...
Embodiment 3
[0092] Carry out experiment with reference to the sample and operation method of 3.1 of embodiment 1, difference is that mobile phase is methyl alcohol: acetonitrile=5:95 (add 50mmol formic acid and 25mmol diethylamine in mixed solution, account for 0.45% of mobile phase volume ). Obtain high-efficiency chromatograms, the results are as follows:
[0093]
[0094] Among them, peak number 1 is maleic acid; peak number 2 is R-timolol; peak number 3 is S-timolol.
[0095] The results show that the chromatographic conditions can effectively separate S-timolol, R-timolol and maleic acid, and the peak shape is better, the baseline is more stable, and the resolution is greater than 1.5.
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