Method for determining genotoxic impurities in doxofylline bulk drugs
A determination method and genotoxicity technology are applied in the field of determination of genotoxic impurities in doxofylline raw materials, and achieve the effects of reducing the loss of fixative solution, purifying test background and ensuring accuracy
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[0092] Example 1:
[0093] 1) Sample preparation:
[0094] Mixed standard series solution preparation: accurately weigh the appropriate amount of each reference substance, and use N,N-dimethylformamide to prepare a vinyl acetate concentration of 3.846mg / ml, 2-bromo-1,1-dioxyethane concentration Single reference substance stock solution of 0.3167mg / ml, respectively accurately measure 1ml of single reference substance stock solution into the same 100ml volumetric flask, add N,N-dimethylformamide to dilute and dilute to the mark to make a mixed control The stock solution of the product, and then accurately draw the appropriate amount of the stock solution of the mixed reference substance, and dilute it to the vinyl acetate concentration of 0.769μg / ml, 1.23μg / ml, 1.54μg / ml, 1.92μg / ml, 2.31μg / ml, 2- Bromo-1,1-dioxyethane concentration is 0.0633μg / ml, 0.101μg / ml, 0.127μg / ml, 0.158μg / ml, 0.190μg / ml mixed standard series solutions;
[0095] Preparation of test product: accurately weigh out...
Example Embodiment
[0108] Example 2-7
[0109] Except for the preparation of the test product using the following method, the same measurement conditions and procedures as in Example 1 were used.
[0110] Preparation of the test product: accurately weigh out the crude and finished doxofylline (provided by Shaanxi Bosen Biopharmaceutical Co., Ltd.) 0.3g into a 10ml volumetric flask, add an appropriate amount of N,N-dimethylformamide, shake and mix well , Seal and ultrasonic for 1min until the sample is completely dissolved, add N,N-dimethylformamide to volume, shake well, pass through a 0.22μm filter membrane, and use the filtrate as the test sample.
[0111] The measured gas chromatogram is as image 3 Shown. image 3 It is the gas chromatography-mass spectrometry analysis pattern of the sample.
[0112] The content determination results of the samples are shown in Table 2-7 below.
[0113] Table 2 Sample content determination results
[0114]
[0115] Table 3 Sample content determination results
[0116] ...
Example Embodiment
[0127] Example 3 Methodological investigation
[0128] The methodological investigation of the specificity, linearity, precision, repeatability, accuracy, stability, detection limit and quantification limit of the two genotoxic impurities in doxofylline bulk drug was carried out. The specific inspection methods are:
[0129] 1. Linear investigation
[0130] Precisely weigh the appropriate amount of each reference substance, and use N,N-dimethylformamide to prepare vinyl acetate with concentrations of 0.769μg / ml, 1.23μg / ml, 1.54μg / ml, 1.92μg / ml, 2.31μg / ml, respectively , 2-bromo-1,1-dioxyethane concentration of 0.0633μg / ml, 0.101μg / ml, 0.127μg / ml, 0.158μg / ml, 0.190μg / ml mixed standard series solution (incremental concentration The sequence is abbreviated as std1 solution, std2 solution, std3 solution, std4 solution and std5 solution). Inject the mixed standard series solution into the gas chromatography-mass spectrometer, measure the corresponding peak area, use the concentration o...
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