Quality control method of process for synthesizing glucurolactone
A technology of glucuronolactone and quality control method, applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of difficult determination of the reaction end point, many by-products, low yield and the like, so as to avoid overreaction or underreaction. , reduce the generation of by-products, and the effect of method specificity is good
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Embodiment 1
[0041] Embodiment 1 glucoside content determination
[0042] 1. Solution preparation
[0043] 1) Preparation of mobile phase: 0.00625mol / L sulfuric acid solution
[0044] 2) Preparation of sample solution: Take about 50 mg of glucoside sample, weigh it accurately, put it in a 50 ml volumetric flask, add water to dissolve and dilute to the mark, shake well, and you get it.
[0045] 3) Preparation of standard solution: take 50mg of glucoside reference substance (dried under reduced pressure at 80°C ± 2°C for 2 hours), weigh it accurately, put it in a 50ml measuring bottle, add water to dissolve, dilute to the mark with water, shake Uniform, as the reference solution.
[0046] 2. Determination method: Take the reference substance solution, inject 20 μl of sample, record the chromatogram, the number of theoretical plates should not be less than 3000 based on the peak of glucoside, and the symmetry factor should be 0.8-1.5. Take 20 μl of the above solution and inject it into a l...
Embodiment 2
[0090] The monitoring of the end point of embodiment 2 glucoside oxidation reaction
[0091] 1. Solution preparation
[0092] 1) Preparation of mobile phase: 0.00625mol / L sulfuric acid solution
[0093] 2) Test solution: (newly prepared for use) During the reaction, take 1g of the oxidation reaction solution, put it in a 50ml measuring bottle, add an appropriate amount of mobile phase to dilute to the mark, shake well, and you get it.
[0094] 2. Measurement method
[0095] Take 20 μl of the test solution and inject it into the liquid chromatograph, record the spectrum, calculate the remaining content of glycoside according to the area normalization method, and judge whether the reaction end point is reached by the remaining amount of glycoside.
[0096] 3. Measurement results
[0097] At the beginning of the reaction, glucoside has two isomers, α and β. The total amount of these two isomers is about 95%. At this point there is no glucoside oxide (see figure 1 ).
[009...
Embodiment 3
[0103] Embodiment 3 Monitoring of the end point of hydrolysis reaction of glucoside methyl oxide
[0104] 1. Solution preparation
[0105] 1) Preparation of mobile phase: 0.00625mol / L sulfuric acid solution
[0106] 2) Test solution: (newly prepared for use) During the reaction, take 1g of the oxidation reaction solution, place it in a 50ml measuring bottle, add an appropriate amount of mobile phase to dilute to the mark, shake well, filter it with a 0.45um filter membrane, and take the continuation The filtrate was used as the test solution.
[0107] 2. Measurement method
[0108] Take 20 μl of the test solution and inject it into a liquid chromatograph, record the spectrum, calculate the remaining content of glucose methyl glycoside oxide by the area normalization method, and judge whether the reaction end point is reached by the remaining amount of methyl glycoside.
[0109] 3. Measurement results
[0110] At the beginning of the reaction, due to the process step of con...
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