A kind of high-performance liquid chromatography method for determining the related substances of Nicergoline
A high-performance liquid chromatography, nicergoline technology, applied in the field of drug analysis, can solve problems such as difficult to obtain, expensive impurity reference substance, unstable impurity retention time and the like
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Embodiment 1
[0074] Example 1 Verification of Chromatography Conditions
[0075] Columns: fillers mixed with strong cation exchange resins and inverted C18 by volume ratio 1: 4;
[0076] Mobile phase: Take acetonitrile as a mobile phase A, phosphate buffer (60 mmol / L of a phosphate solution containing 0.5% triethylamine, pH value to 2.1) as a mobile phase B. The mobile phase A, the mobile phase B is eluted at a ratio of 30:70;
[0077] Test wavelength: 288 nm;
[0078] Column temperature: 30 ° C;
[0079] Preparation of impurity test solution: Take an EP system applicability, 1 ml of acetonitrile is precisely added to dissolve.
[0080] Preparation of mixed impurities Takes: Take impurities D 9.42mg, impurity A (chloromye forest) 10.68 mg, impurity G (1-demetalloxinin forest) 10.25mg, impurity B (1 - Nikhene 10.30 mg, 10.30 mg of impurity C, respectively, in 10 ml of volumetric flask, dissolved with acetonitrile and diluted to the scale, as the liquid reserve solution. Take 1 ml, 2.5 mL, 2.5...
Embodiment 2
[0085] Example 2 Ni Mimum Lin Heat Stability Investigation
[0086] Precision is called 0.1028 g of Niwheneflin, and in a 100 mL volumetric flask, add acetonitrile-water (8: 2) to dissolve and dilute to the scale, shake well as a test solution. The test solution was taken at a 60 ° C water bath to heat the damage, and 20 μl of heat 0min, 10 min, 30 min, 50 min, respectively, 20 μl of the liquid chromatography, and the chromatographic chart of Example 1, see the chromatogram. Figure 4 ~ 7 The result indicates that Ni Mailin forest is thermally degraded, and impurity D and impurity C gradually increase with heating time, in particular, see Table 1.
[0087] Table 1
[0088]
Embodiment 3
[0089] Example 3 Linear range, detection limit and quantitative limit
[0090] Take impurities D 9.42mg, impurity A (chloroni-necrhable forest) 10.68mg, impurity G (1-demethoxide forest) 10.25 mg, impurity B (1-Nikhenechelin) 10.30mg, impurity C 10.30, The Ni Mikin forest was 10.12 mg, and in 10 ml of volumetric flask, the Nika, which was dissolved with acetonitrile and diluted to the scale, as each pair of object reserves. The appropriate amount of each paternal reserved solution was obtained separately, and a series of concentrations of solution was diluted with acetonitrile, and the chromatographic conditions of Example 1 were respectively injected into a liquid chromatograph, and the chromatogram is recorded. Take concentration (μg · ml -1 The linear regression equation and correction factor of each component is calculated as X, and the ratio of the linear regression equation and the correction factor of each component is calculated (the ratio of Ni Mai Linlin slope), and the ...
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