HPLC analysis method of 4-nitrophenylethylamine
A technology of nitrophenethylamine and an analytical method, applied in the field of pharmaceutical analysis, can solve problems such as inability to effectively distinguish impurities, interference of determination results of content, and achieve reliable content determination and impurity control, high sensitivity and accuracy, and specificity. Good results
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Embodiment 1
[0055] Detection method:
[0056] Take an appropriate amount of 4-nitrophenylethylamine test sample, accurately weighed, add 10% acetonitrile to dissolve and dilute to a 0.2mg / ml sample solution, shake well, accurately measure 10 μl and inject it into the liquid chromatograph, at a flow rate of 1.0ml / Min and column temperature of 25 ° C for HPLC analysis, record the chromatogram.
[0057] The concentration of potassium dihydrogen phosphate buffer in mobile phase A is 0.01mol / L, the pH is 2.0, and the proportion of acetonitrile is 10%.
[0058] Analyze the system suitability solution according to the following gradient elution procedure
[0059] time (min) Mobile phase A% Mobile phase B% 0 100 0 5 100 0 10 80 20 15 80 20 16 100 0 23 100 0
[0060]Chromatogram see figure 1 , the retention time of each impurity and the main peak and the resolution between adjacent peaks are shown in Table 2.
[0061] Table 2 Retention tim...
Embodiment 2
[0065] Others are the same as embodiment 1, the difference is:
[0066] The concentration of potassium dihydrogen phosphate buffer in mobile phase A is 0.005mol / L or 0.05mol / L;
[0067] Analyze the system adaptability solution according to the gradient elution program in Example 1, see the chromatogram figure 2 and 3 , the retention time of each impurity and the main peak and the resolution between adjacent peaks are shown in Table 3 and Table 4.
[0068] The separation result when the concentration of potassium dihydrogen phosphate buffer solution in mobile phase A in table 3 is 0.005mol / L
[0069] name / code retention time (min) Resolution between adjacent peaks Impurity A 2.672 / Impurity D 3.138 4.2 Impurity E 4.159 8.4 4-Nitrophenethylamine 4.392 1.2 Impurity B 10.131 28.0 Impurity C 11.697 12.5
[0070] The separation result when the potassium dihydrogen phosphate buffer concentration is 0.05mol / L in the mobi...
Embodiment 3
[0075] Others are the same as embodiment 1, the difference is:
[0076] The pH of potassium dihydrogen phosphate buffer in mobile phase A is 1.5 or 3.0;
[0077] Analyze the system adaptability solution according to the gradient elution program in Example 1, see the chromatogram Figure 4 and 5 , the retention time of each impurity and the main peak and the resolution between adjacent peaks are shown in Table 5 and Table 6.
[0078] The separation result when the pH of potassium dihydrogen phosphate buffer solution in table 5 mobile phase A is 1.5
[0079] name / code retention time (min) Resolution between adjacent peaks Impurity A 2.804 / Impurity D 3.335 4.6 Impurity E 4.452 8.5 4-Nitrophenethylamine 4.742 1.5 Impurity B 10.510 30.9 Impurity C 11.972 12.3
[0080] The separation result when the pH of potassium dihydrogen phosphate buffer solution in table 6 mobile phase A is 3.0
[0081] name / code ret...
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