Quality inspection method for glycoside sulfonyl succinate product by using content of maleic anhydride and sulfonating rate as indexes
A technology of glycoside sulfosuccinate and maleic anhydride, which is applied in the field of quality inspection of glycoside sulfosuccinate salt products, can solve large errors and uncertainties, cannot directly reflect the quality of intermediates and sulfonation rate, It is difficult to achieve higher quality control goals and other issues, to achieve objective and accurate analysis results, and to overcome errors and uncertainties
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[0030] Example 1
[0031] C 8-10 The sodium alkyl glycoside sulfosuccinate product has the following structure:
[0032]
[0033] It is sulfonated with the following intermediates and sodium sulfite aqueous solution:
[0034]
[0035] Where R stands for C 8 -C 10 的linear alkyl group; w is 0; k is 1.2; X 1 for X 3 , X 4 Is H, M is Na + ; Y 1 Is -COCH=CHCOOH, Y 2 , Y 3 , Y 4 For H.
[0036] The quality inspection method is as follows:
[0037] (1)C 8-10 After the synthesis of the alkyl glycoside maleate intermediate is completed, take a sample, add water to dissolve it, and use it as an intermediate sample to be tested for analysis on a high performance liquid chromatograph. The chromatographic conditions are: 8 Chromatographic column; methanol:water mixed solvent with a volume ratio of 5:95 as the mobile phase, adding 0.01% trifluoroacetic acid in volume ratio before use; UV detector detection, detection wavelength 214nm. Using maleic anhydride as the reference substance, the content ...
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[0046] Example 2
[0047] Carbon chain is C 12-14 The product of potassium alcohol ether glycoside sulfosuccinate with ethylene oxide adduct number of 2 has the following structure:
[0048]
[0049] It is sulfonated with the following intermediates and sodium sulfite aqueous solution:
[0050]
[0051] Where R stands for C 12 -C 14 的Straight-chain alkyl; w is 2; k is 3.5; X 1 , X 2 for X 3 , X 4 Is H, M is K + ; Y 1 , Y 2 Is COCH=CHCOOH, Y 3 , Y4 is H.
[0052] The quality inspection method is as follows:
[0053] (1) The carbon chain is C 12-14 , After the synthesis of the alcohol ether glycoside maleate intermediate with ethylene oxide adduct number of 2, take a sample, add water to dissolve it, and use it as an intermediate sample to be tested and perform analysis on a high performance liquid chromatograph. The chromatographic conditions are : C 18 Chromatographic column; acetonitrile:water mixed solvent with a volume ratio of 15:85 as the mobile phase, adding 0.5% phosphoric aci...
Example Embodiment
[0061] Example 3
[0062] Carbon chain is C 16-18 The ammonium alcohol ether glycoside sulfosuccinate product with an ethylene oxide adduct number of 3 has the following structure:
[0063]
[0064] It is sulfonated with the following intermediates and sodium sulfite aqueous solution:
[0065]
[0066] Where R stands for C 16 -C 18 的linear alkyl group; w is 3; k is 2.4; X 1 , X 2 , X 3 for X 4 Is H, M is NH 4 + ; Y 1 , Y 2 , Y 3 Is COCH=CHCOOH, Y 4 For H.
[0067] The quality inspection method is as follows:
[0068] (1) The carbon chain is C 16-18 After the synthesis of the alcohol ether glycoside maleate intermediate with the ethylene oxide adduct number of 3 is completed, take a sample, add water to dissolve it, and use it as an intermediate sample to be tested. The analysis operation is performed on a high performance liquid chromatograph. The chromatographic conditions are : C 8 Chromatographic column; acetonitrile:water mixed solvent with a volume ratio of 20:80 as the mobile p...
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