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Preparation method for semicarbazide hydrochloride labeled by stable isotope 13C and 15N

A technology of semicarbazide hydrochloride and isotope, which is applied in the field of preparation of stable isotope 13C and 15N labeled semicarbazide hydrochloride, can solve the problems of high price and late start, and improve product quality, reduce production cost, food The effect of improving the level of safety inspection

Active Publication Date: 2010-08-25
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing isotope types are mainly concentrated in the fields of biology, chemical minerals, etc., and the stable isotope veterinary drugs related to food testing started relatively late, and all of them need to be imported from abroad, which is expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a stable isotope 13 C and 15 The preparation method of N label semicarbazide hydrochloride, the method comprises the following steps:

[0022] (1) 15 N 2 -N 2 h 4 ·H 2 Preparation of O

[0023] 62g of available chlorine containing 12wt% NaClO solution was added dropwise to 2g anhydrous magnesium sulfate, 6.6g 15 N-labeled urea ( 15 N 2 -Urea), 10g NaOH and 10ml deionized water solution, at this time 15 N 2 -The molar ratio of Urea, NaClO and NaOH is 1.1:1:2.5. The temperature was controlled at 80°C by an oil bath, and after 3 hours of reaction, the crude 15 N 2 -N 2 h 4 ·H 2 The synthetic solution of O is determined by GC in this synthetic solution 15 N-N 2 h 4 ·H 2 The content of O is 4.6%, thus can calculate this step reaction to obtain 15 N 2 -N 2 h 4 ·H 2 The O yield is 78%, and the insoluble matter in the synthetic solution is filtered out by anhydrous magnesium sulfate, and the filtrate is collected, and the filtrate is allowed to stand at...

Embodiment 2

[0027] Adopt the same operation step as embodiment 1, just the step (1) in 15 N 2 -The molar ratio of Urea, NaClO and NaOH is changed to 1.2: 1: 2.7, namely adding 7.2g 15 N 2 -Urea, 10.8g NaOH and 62g containing available chlorine are 12wt% NaClO solution, the reaction temperature and the reaction time are constant. obtained by this reaction 15 N 2 -N 2 h 4 ·H 2 The O yield was 69%. Step (2) is also the same as in Example 1, except that the temperature of reaction in step (2) is changed to 120° C., and the reaction time is constant. obtained by this reaction 13 C, 15 N 3 - The yield of SEM·HCl crystals was 85%.

Embodiment 3

[0029] a stable isotope 13 C and 15 The preparation method of N label semicarbazide hydrochloride, the method comprises the following steps:

[0030] (1) 15 N 2 -N 2 h 4 ·H 2 Preparation of O

[0031] Will 15 N-labeled urea ( 15 N 2 -Urea), NaClO and NaOH are mixed in a molar ratio of 1.05: 1: 2.3, the reaction temperature should be controlled at 70°C, and react for 8 hours under the catalysis of catalyst anhydrous magnesium sulfate and gelatin, the weight of the catalyst is 1 / 4 of NaOH, The mass fraction of available chlorine in NaClO is 9%. After the reaction is over, the mother liquor is filtered to remove the catalyst insoluble in the mother liquor. 2 CO 3 , after high-speed centrifugation, the supernatant was collected, and the obtained supernatant was purified by vacuum distillation. The temperature of the distilled water bath was controlled at 30°C, and the system was evacuated by a rotary vane vacuum pump. The distillation time was 6h. After vacuum distillat...

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Abstract

The invention relates to a preparation method for semicarbazide hydrochloride labeled by stable isotope 13C and 15N. The method comprises the following steps that: after urea labeled by 15N, NaClO and NaOH are mixed, catalyzed and filtered, liquid supernatant is collected and distilled under reduced pressure to obtain 15N2-N2H4.H2O solution, the obtained 15N2-N2H4.H2O solution is mixed and reacts with urea labeled by 13C and 15N, concentration and dehydration are conducted and pH value is regulated, and after concentration is conducted again to remove ionized water, recrystallization is conducted to obtain semicarbazide containing stable isotope. Compared with the prior art, the invention fills the blank in the preparation of stable isotope internal standard reagent required in the testing of veterinary drug residue metabolite in China, and has the advantages that the production cost is reduced, the product quality is improved, the high-abundance isotope internal standard reagent with small abundance drop value is obtained by the high utilization ratio of 13C and 15N, and the method is an internal standard substance preparation and purification method which is badly needed in food safety testing.

Description

technical field [0001] The present invention relates to a kind of preparation method of semicarbazide hydrochloride, especially relate to a kind of stable isotope 13 C and 15 The preparation method of N-labeled semicarbazide hydrochloride. Background technique [0002] After the globalization of the world economy and China's accession to WTO, trade and technical exchanges between China and other countries in the world have become increasingly frequent, and the reliability of food safety analysis and measurement has become increasingly important, and the requirements have become higher and higher. Substances such as antibiotics, sulfonamides, furans, anticoccidials, hormones and anthelmintics may remain in food of animal origin and endanger human health. Because furan drugs can be rapidly metabolized and are not easily detected in edible animal tissues, it is not suitable to detect the residues of furan drugs by determining the parent compound. Because mass spectrometry ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C281/06
Inventor 王伟杜晓宁刘占峰徐建飞王刚张亮宋明鸣
Owner SHANGHAI RES INST OF CHEM IND
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