Method for separating carbamazepine and its related substances through liquid chromatography
A carbamazepine and liquid chromatography technology, which is applied in the field of liquid chromatography to separate carbamazepine and related substances, can solve the problem that the sensitivity of the method is insufficient, the signal-to-noise ratio of impurity E cannot meet the verification conditions, the sensitivity of impurity E is low, etc. question
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experiment example 1
[0104] Experimental Example 1: Verification of Chromatographic Conditions in Pharmacopoeia
[0105] According to the chromatographic conditions stipulated in the Chinese Pharmacopoeia, a system adaptability experiment was carried out on carbamazepine, and the carbamazepine sample used was produced by our company with batch number 2017021303. The specific chromatographic conditions are as follows:
[0106] (1) Chromatographic conditions
[0107]
[0108] (2) Sample preparation
[0109]
[0110]
[0111] (3) See the results figure 1 . The separation of carbamazepine and impurity A, impurity B, impurity C, impurity D and impurity E is as follows.
[0112] name
keep time
area
Number of theoretical plates
Separation
Impurity B
9.153
439898
3861
58.06
Impurity A
12.379
162994
3594
4.70
15.93
carbamazepine
14.193
8501116
3802
2.13
725.00
Impuri...
Embodiment 1
[0132] Embodiment 1: the exploratory test of carbamazepine related substance detection condition
[0133] 1. First, change the mobile phase system. There is tetrahydrofuran in the mobile phase system, which has absorption at low wavelengths, which may cover up the impurity peaks, and adopt the acetonitrile-water gradient elution method. The new chromatographic conditions are as follows:
[0134] (1) Chromatographic conditions
[0135]
[0136] (2) See the attached chromatogram for the results Figure 5 . Carbamazepine and the separation of impurities are as follows:
[0137]
[0138] (3) Conclusion
[0139] The concentration of each impurity in carbamazepine was about 9 μg / mL, one impurity in carbamazepine did not appear as a peak, and the other impurities were well separated. Reason analysis: In addition to removing tetrahydrofuran from the mobile phase, triethylamine was removed at the same time, and the impurity of carbamazepine contains N, so there is no peak. ...
Embodiment 2
[0200] Embodiment 2 Destructive test
[0201] 1 Acid, alkali and oxidation damage (sample group: 2017032801)
[0202] 1.1 Undestroyed API
[0203] Take 75 mg of carbamazepine raw material, accurately weigh it, put it in a 50 ml measuring bottle, add 25 ml of methanol to dissolve, ultrasonically dissolve, add water to dilute to the mark, shake well, and obtain. Measure 5.00ml of the solution in a 50ml volumetric flask, add 22ml of methanol, dilute with water to the mark, and shake well to obtain.
[0204] see attached results Figure 17 :
[0205] name
keep time
peak name
Purity angle
Purity Threshold
area
area%
Separation
s / n
1
21.338
main peak
0.232
0.345
52876503
100
12862.92
[0206] 1.2 Acid Destruction
[0207] Acid-base blank: Pipette 5.00ml of 1mol / L hydrochloric acid solution and sodium hydroxide solution into a 50ml volumetric flask, add 25ml of methanol solution, dilute with water to t...
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