Method for detecting organic impurities in 2-vinylpyridine
A technique for vinylpyridine, organic impurities, applied in the field of analytical chemistry
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Embodiment 1
[0037] Embodiment 1 chromatographic conditions
[0038] Selection of dissolution medium: Both the analyte and the sample have good solubility in water, so water is selected as the solvent.
[0039] Selection of chromatographic column and column temperature: According to the boiling point and polarity of the analyte, select a capillary column with polyethylene glycol as the stationary liquid, and the initial temperature is 60°C.
[0040] Chromatographic conditions and system suitability test: according to gas chromatography, using a capillary column of DB-WAXETR (60m×0.32mm×0.5μm), the initial temperature is 60°C, maintained for 2 minutes, and the temperature is raised to 12°C per minute. 260°C for 15 minutes; the temperature of the injection port is 320°C; the detector is an FID detector, and the temperature of the detector is 320°C; the carrier gas is nitrogen; the column flow rate is 3.0ml / min; the split ratio is 1:1.
[0041] Accurately weigh about 0.1g of each impurity 1-...
Embodiment 2
[0042] Embodiment 2 methodological verification
[0043] Table 2 Methodology Validation
[0044]
[0045] 2.1 Specificity
[0046] Take the blank solvent and the mixed reference solution, and inject the sample. The results showed that the blank solvent did not interfere with the detection, and the separation between the chromatographic peaks of each component was greater than 1.5, and the specificity of the method was good.
[0047] 2.2 Linear relationship
[0048] Take an appropriate amount of impurities 1-8, prepare impurity reference substance stock solution according to the preparation method of reference substance solution, and quantitatively dilute step by step, as a linear reference substance solution.
[0049] With the concentration as the abscissa and the peak area as the ordinate, a linear regression is performed, and the results are shown in the table below.
[0050] Table 3 Linearity and range test results
[0051]
[0052] 2.3 Limit of detection and lim...
Embodiment 3
[0096] Example 3 Sample Determination
[0097] 3.1 According to the methodological research data, the detection method for determining impurities 1-8 is:
[0098] Chromatographic conditions and system suitability test: according to gas chromatography, using a capillary column of DB-WAXETR (60m×0.32mm×0.5μm), the initial temperature is 60°C, maintained for 2 minutes, and the temperature is raised to 12°C per minute. 260°C for 15 minutes; the temperature of the injection port is 320°C; the detector is an FID detector, and the temperature of the detector is 320°C; the carrier gas is nitrogen; the column flow rate is 3.0ml / min; the split ratio is 1:1.
[0099] Accurately weigh about 0.1g of each impurity 1-8, put it in a 100ml measuring bottle, dilute with water to the mark, shake well, and use it as the impurity stock solution, precisely measure 1ml of each impurity stock solution, put it in a 100ml measuring bottle, dilute with water to the mark, shake Evenly, as the reference ...
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