Analysis method for lamivudine related substance inspection
A technology for lamivudine and related substances, which is applied in the analysis field of separation and determination of lamivudine and its various known impurities by liquid chromatography, and can solve the problem of separation of non-degradable peaks and known impurities and failure to detect Degradation peaks and other problems, to achieve the effect of accurate quality and accurate determination
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Embodiment 1
[0056] Instruments and conditions:
[0057] Shimadzu LC-10AD / SIL-10AD / SPD-M10A / SCL-10A / DGU-14A high-performance liquid chromatography and Shimadzu's workstation; use alkaline deactivated octadecylsilane bonded silica gel as filler (BDS HYPERSIL C 18 , 4.6mm×25cm×5μm, THERMO); with 1.9g / L ammonium acetate solution (take 1.9g of ammonium acetate, add about 900ml of water to dissolve, shake well, adjust the pH value to 3.8 with glacial acetic acid, add water to dilute to 1000ml) as Mobile phase A, with methanol as mobile phase B; detection wavelength is 277nm; column temperature is 35°C. Mobile phase flow rate: 1.0ml / min, liquid phase analysis injection volume: 10μl; gradient elution according to the following table:
[0058] time (min)
Mobile phase A(%)
Mobile phase B(%)
0
97
3
30
97
3
45
70
30
60
70
30
63
97
3
73
97
3
[0059] experiment procedure:
[0060] Take...
Embodiment 2
[0074] Basically the same method as in Example 1, the difference is that when preparing the mobile phase A, it is prepared into different pH values, and then the high-temperature degradation solution is detected according to the method in Example 1 to detect the number of impurities and all The minimum separation between any two adjacent chromatographic peaks in the chromatographic peak is the index, and the separation effect of mobile phase A with different pH values in gradient elution is investigated, and the injection volume is 20ul. The result is as follows:
[0075] pH of mobile phase A
[0076] For the high-performance liquid chromatography analysis method of drugs, those skilled in the art know that generally speaking, the acceptable separation generally needs to be above 1.0, and usually when the separation degree is greater than 1.5, it is considered that the standard required by the quality control method can be met. The present inventors have found that...
Embodiment 3
[0078] Basically the same method as in Example 1, the difference is that different chromatographic column temperatures are measured when separating, and the high-temperature degradation solution is detected according to the method in Example 1, with the number of impurities detected and any of the total chromatographic peaks The minimum value of the separation between two adjacent chromatographic peaks is an index, and the separation effect of mobile phase A with different pH values in gradient elution is investigated, and the results are as follows:
[0079] Column temperature (°C)
[0080]The present inventors have found that, in the process of using gradient elution, when the column temperature of the chromatographic column is in the range of 33 to 37, not only the resolution is good, but also the most impurities can be detected; , the detectable impurities are reduced, and the resolution between them cannot meet the general analysis requirements; and when the co...
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Abstract
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