Liquid chromatographic analysis method for detecting content of rearranged ester
A technology of liquid chromatography analysis and liquid chromatography, which is applied in the field of liquid chromatography analysis to detect the content of rearranged esters, can solve the problems of complex response factor gap of product impurities, unclear chromatographic conditions, etc., and achieve short analysis time, heavy Good performance and good peaking effect
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[0058]Example 1
[0059]1.1 Reagents and instruments
[0060]Methanol: HPLC;
[0061]Rearrangement ester standard sample: self-made purity 98.9%;
[0062]Analytical balance: 0.0001g;
[0063]Organic phase microporous membrane: 0.22μm;
[0064]Liquid chromatograph: U3000, Thermo Fisher Scientific, equipped with UV detector, equipped
[0065]Autosampler;
[0066]Capillary chromatography column: C18 liquid chromatography column, 150mm×4.6mm×2.6μm, Thermo
[0067]Flying company
[0068]1.2 Chromatographic method
[0069]a) Mobile phase: A: Acetonitrile or methanol; B: 1% phosphoric acid or acetic acid aqueous solution
[0070]b) Flow ratio example A:B=80:20;
[0071]c) Injection volume: 20.0μL;
[0072]d) Column thermostat: 30℃;
[0073]e) Flow rate: 1mL / min;
[0074]f) Detection type: UV detector;
[0075]g) Detection wavelength: 222nm;
[0076]h) Chromatographic column: C18 liquid chromatography column, 150mm×4.6mm×2.6μm;
[0077]1.3 Draw a standard curve
[0078]Take standard working fluids respectively, and carry out chromatographic analysis...
Example Embodiment
[0092]Example 2
[0093]Example 2 includes most of the technical features of Example 1. The difference from Example 1 is that the sampling position in Example 2 is the raw material for the production process, and about 70% of the material is rearranged esters, so the pretreatment The method is as follows: Take 1.0258g sample, add the mobile phase to a 100mL volumetric flask, and shake it up as the sample stock solution, then remove 1mL of the sample stock solution and dilute with mobile phase to a constant volume in a 100mL volumetric flask. Use a 0.22μm filter membrane Sample injection analysis after filtration.
[0094]The analysis chromatogram of this example is asFigure 4 According to this method, the content of rearranged ester is 69.511%.
[0095]Among them, inFigure 2-Figure 4The vertical axis represents absorbance or absorptivity, inFigure 2-Figure 4It is represented by Absorbance.
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