Title:
METHOD FOR DETERMINING AMOUNTS OF GLYCINE AND DIKETOPIPERAZINE IN REACTION LIQUID BY USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY
Document Type and Number:
WIPO Patent Application WO/2024/109016
Kind Code:
A1
Abstract:
A method for measuring the yield of a synthetic product diketopiperazine in a reaction process of synthesizing diketopiperazine from glycine by using high performance liquid chromatography in the field of chemical testing and analysis. The method comprises: mixing 700 mL of methanol with 300 mL of water as a mobile phase, adding an ion pair reagent tetrabutylammonium bromide as a stabilizer, regulating the pH value to be about 5.0 by using potassium dihydrogen phosphate as a buffer salt, and separating and determining the amounts of glycine and diketopiperazine by using a Waters Anionic Polar Pesticide chromatographic column. The reaction raw material glycine has weak ultraviolet absorption under the same wavelength in the reaction process, and the polarity of glycine is similar to that of the product diketopiperazine, so that the phenomena of similar retention time, peak overlapping and poor detection stability as the reaction product increases occur. By adjusting liquid chromatography conditions, the amounts of glycine and diketopiperazine can be rapidly and accurately determined, and timely and accurate data guidance is provided for adjustment of production process parameters of synthesis of diketopiperazine from glycine.
Inventors:
RONG SHASHA (CN)
DU JIANXIA (CN)
LI HONG (CN)
XIAO QINGYAN (CN)
LU HUIZHEN (CN)
YU XIAOYING (CN)
CHAO YUHUI (CN)
CAO HONGYAN (CN)
XU WEI (CN)
DU JIANXIA (CN)
LI HONG (CN)
XIAO QINGYAN (CN)
LU HUIZHEN (CN)
YU XIAOYING (CN)
CHAO YUHUI (CN)
CAO HONGYAN (CN)
XU WEI (CN)
Application Number:
PCT/CN2023/102368
Publication Date:
May 30, 2024
Filing Date:
June 26, 2023
Export Citation:
Assignee:
HUBEI THREE GORGES LABORATORY (CN)
International Classes:
G01N30/28; G01N30/02; G01N30/34
Domestic Patent References:
| WO2011075002A1 | 2011-06-23 |
Foreign References:
| CN106596799A | 2017-04-26 | |||
| CN107091891A | 2017-08-25 | |||
| CN107621507A | 2018-01-23 | |||
| CN112924566A | 2021-06-08 | |||
| CN115201363A | 2022-10-18 |
Other References:
SAKATA KASUMI, YABUTA HIKARU; KONDO TADASHI: "Effects of metal ions and pH on the formation and decomposition rates of di- and tri-peptides in aqueous solution", GEOCHEMICAL JOURNAL, GOYA UNIVERSITY, vol. 48, no. 2, 1 January 2014 (2014-01-01), pages 219 - 230, XP093175152, ISSN: 0016-7002, DOI: 10.2343/geochemj.2.0300
Attorney, Agent or Firm:
YICHANG THREE GORGES PATENT (CN)
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