The purity analysis method of Methyl Ergoline Acid
1.1. Purity
Instrument：Liquid chromatograph，Electronic balance (Hundred thousandth).
Reagents：Acetonitrile(HPLC)，Pure Water(Pure 0.45μm membrane filtration)，Ammonium formate.
1.1.1Chromatographic Conditions
|
Chromatographic Column |
C184.6x250mm, 5μm or equivalent chromatographic columns |
|
Detection Wavelength |
254nm |
|
Column Temperature |
30℃ |
|
Flow Velocity |
1.0ml/min |
|
Injection Volume |
20μL |
|
Mobile Phase A |
0.2mol/L Ammonium formate(Weigh 12.6g of ammonium formate and dissolve it in 1000ml of purified water, then filter it through a 0.45 μ m membrane and degas it with ultrasound for 30 minutes.) |
|
Mobile Phase B |
Acetonitrile |
Time program：
|
Time(minute) |
Mobile phase A(%) |
Mobile phase B(%) |
|
0 |
90 |
10 |
|
10 |
85 |
15 |
|
13 |
58 |
42 |
|
25 |
58 |
42 |
|
30 |
0 |
10 |
|
31 |
90 |
10 |
|
36 |
90 |
10 |
1.1.2. Solution Formulation
Blank solution：Acetonitrile
Test solution：Take approximately 30mg of the test sample, weigh it accurately, place it in a 50ml volumetric flask, dissolve it in acetonitrile, dilute to the mark, shake well, and prepare two test sample solutions in parallel.
According to the above chromatographic conditions, after the system stabilizes, inject the sample according to the following sequence table.
|
Sample Name |
Injection frequency |
|
Blank solution |
≥1 |
|
Test solution 1 |
1 |
|
Test solution 2 |
1 |
1.1.3. Acceptance criteria
Calculate the relative percentage content of the main peak using the peak area normalization method, and the purity should not be lower than 97.0%.
