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Stable isotope labeled ethyl 3-aminobenzoate-d 5 and its preparation method

An aminobenzoic acid and isotope labeling technology, which is applied in the direction of isotope introduction into organic compounds, acyclic/carbocyclic compound isotope introduction, organic chemical methods, etc., can solve the problems of high detection limit of high performance liquid chromatography and spectrophotometry, and achieve The process route is simple, the promotion prospect is good, and the effect of easy separation and purification

Active Publication Date: 2021-10-15
CHINESE ACAD OF FISHERY SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

HPLC and spectrophotometry have high detection limits and are rarely used

Method used

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  • Stable isotope labeled ethyl 3-aminobenzoate-d <sub>5</sub> and its preparation method
  • Stable isotope labeled ethyl 3-aminobenzoate-d <sub>5</sub> and its preparation method
  • Stable isotope labeled ethyl 3-aminobenzoate-d <sub>5</sub> and its preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Measure 5mL (85.6mmol) ethanol-D 6 (DOCD 2 cd 3 ) and 0.5g (3.3mmol) 3-aminobenzoic acid were successively added into the round-bottomed flask; the round-bottomed flask was placed in an ice bath, and under magnetic stirring conditions, 0.5mL thionyl chloride was added dropwise; after completion, the Place the round-bottomed flask at room temperature and continue magnetic stirring for 2 hours; after the reaction is complete, concentrate by rotary evaporation to a volume of about 1 mL; cool to room temperature, add 150 mL of water; add 10 mL of ethyl acetate for extraction, repeat the extraction three times, and combine ethyl acetate for extraction solution; add 50mL water to wash the ethyl acetate extract, and repeat the washing three times; after concentrated by rotary evaporation, use silica gel chromatography column for separation and purification to obtain stable isotope labeled ethyl 3-aminobenzoate-D 5 .

[0032] Ethyl 3-aminobenzoate-D by HPLC-MS using ion sour...

Embodiment 2

[0034] 1 Material method

[0035] 1.1 Instrument

[0036] 20At high performance liquid chromatography (Shimadzu), 8060 triple quadrupole mass spectrometer (Shimadzu), etc.

[0037] 1.2 Reagents

[0038] Acetonitrile (chromatographically pure, purchased from Merck, Germany), sodium chloride and anhydrous magnesium sulfate (analytical pure, purchased from Beijing Chemical Plant), PSA (40-63 μm, Purchased from Shanghai Anpu Experiment Technology Co., Ltd.), ethyl 3-aminobenzoate (imported, purity>98%), ethyl 3-aminobenzoate-D 5 (laboratory synthesis), ethyl 3-aminobenzoate and ethyl 3-aminobenzoate-D 5 Standard solutions were prepared in methanol.

[0039] 1.3 Chromatographic conditions

[0040] a) Chromatographic column: Kromasil C18 reverse-phase chromatographic column ((2.1mm×50mm, 3.5μm);

[0041] b) Mobile phase and gradient elution conditions:

[0042]At the end of 0-1.5min, the volume percentage of mobile phase 0.1% formic acid aqueous solution is from 60% to 10%, ...

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Abstract

The invention discloses a stable isotope labeled ethyl 3-aminobenzoate-D5 and a preparation method thereof. The method involves: ethanol‑D 6 It is an isotope-labeled precursor obtained through bimolecular esterification with 3-aminobenzoic acid; the ethanol-D 6 for DOCD 2 cd 3 . The present invention fills up the stable isotope label 3-aminobenzoic acid ethyl ester-D 5 Missing status, prepared stable isotope labeled 3‑aminobenzoic acid ethyl ester‑D 5 The position of the isotope label is stable, and the isotope abundance is above 99.0% atom D, which can fully meet the needs of residual isotope dilution-liquid chromatography tandem mass spectrometry detection in the field of food safety.

Description

technical field [0001] The invention relates to an organic synthesis method of a stable isotope internal standard substance, in particular to a stable isotope labeled ethyl 3-aminobenzoate-D 5 method of preparation. Background technique [0002] In recent years, an aquaculture market in Beijing used anesthetics to transport live fish. After being exposed by the media, the safety of anesthetics has been aroused. MS-222 (3-Aminobenzoic acid ethyl ester methanesulfonate) chemical name is 3-aminobenzoic acid ethyl ester methanesulfonate, cas number 886-86-2, molecular formula is C 10 h 15 NO 5 S, the structural formula is shown in formula a. MS-222 is a fish anesthetic approved by the United States, Canada and Norway for use in the aquatic industry. However, relevant studies have shown that residual MS-222 in aquatic products will cause potential risks to human health after bio-migration and accumulation in the human body, such as allergic reactions, hematopoietic disorders...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/60C07C227/18C07C227/40C07B59/00G01N30/72
CPCC07B59/001C07B2200/05C07C227/18C07C227/40C07C229/60G01N30/7233
Inventor 李晋成韩刚刘欢
Owner CHINESE ACAD OF FISHERY SCI
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