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Sucralose intermediate analysis detection method

A technology of sucralose and detection method, which is applied in the food field and can solve the problems of low sensitivity

Inactive Publication Date: 2012-01-18
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The object of the present invention is to propose a kind of 2,3,4,3',4'-pentaacetyl sucrose (4-PAS) and 2,3,6,3',4'-pentaacetyl sucrose (6-PAS) ) analysis and detection method to overcome the low sensitivity of existing detection methods

Method used

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  • Sucralose intermediate analysis detection method
  • Sucralose intermediate analysis detection method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Dissolve 10 mg of standard 4-PAS or 6-PAS in 1 ml of pyridine, add 0.4 ml of hexamethyldisilazane and 0.2 ml of trimethylchlorosilane, react for five minutes, evaporate to dryness under reduced pressure, add dichloromethane to dissolve, Centrifuge and take the supernatant for GC and GC analysis. The retention time of 4-PAS was 21.164min, and the retention time of 6-PAS was 28.455min.

[0018] Chromatographic conditions: analyzed by Shimadzu GC-2010 gas chromatograph. Chromatographic column: rtx-50, 30m×0.25mm×0.25μm; inlet temperature: 270°C; detector temperature: 280°C; column oven temperature: 250°C; carrier gas is N 2 , flow rate is 0.6ml / min; split ratio: 19:1.

[0019] Gas conditions: Shimadzu GCMS-QP2010 gas chromatography-mass spectrometer was used. Chromatographic column: rtx-5ms, 30m×0.25mm×0.25μm; the temperature of the injection port, detector and column thermostat is consistent with the above gas phase conditions. The carrier gas is He, the flow rate is ...

Embodiment 2

[0021] With reference to embodiment 1 chromatographic conditions.

[0022] Take 10 mg of the synthesized sucralose intermediate sample containing 4-PAS and dissolve it in 1 ml of pyridine, add 0.4 ml of hexamethyldisilazane and 0.2 ml of trimethylchlorosilane, react for five minutes, evaporate to dryness under reduced pressure, add Dichloromethane was dissolved, centrifuged, and the supernatant was taken for gas chromatography and gas chromatography analysis (the retention time of 4-PAS was 21.164min), and the content of 4-PAS obtained quantitatively by the internal standard method was 82%.

Embodiment 3

[0024] With reference to embodiment 1 chromatographic conditions.

[0025] Samples were taken during the reaction of 4-PAS to generate 6-PAS, evaporated to dryness under reduced pressure, dissolved in 1ml of pyridine, added 0.4ml of hexamethyldisilazane and 0.2ml of trimethylchlorosilane, reacted for five minutes, evaporated under reduced pressure Dry, add dichloromethane to dissolve, centrifuge, get the supernatant and carry out gas chromatography analysis (the retention time of 4-PAS is 21.164min; The retention time of 6-PAS is 28.455min), adopt the area normalization method to just can determine 4 The relative content of -PAS and 6-PAS, so that the reaction conditions can be optimized.

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Abstract

The invention discloses an analyzing detection method of sucralose midbody 2,3,4, 3',4'- penta-acetyl sucrose and / or 2,3,6, 3',4'- penta-acetyl sucrose. The technical key point is as follows: the 2,3,4, 3',4'- penta-acetyl sucrose and / or 2,3,6, 3',4'- penta-acetyl sucrose is derived through trimethylsilyl etherification and undergoes qualitative analysis through a gas chromatograph-mass spectrometer and quantitative analysis through gas phase chromatography and obtains good results. The analyzing detection method is applicable to the process control of sucralose synthesis.

Description

technical field [0001] The invention relates to the field of food technology, in particular to sucralose intermediates 2,3,4,3',4'-pentaacetyl sucrose and 2,3,6,3',4'- Analytical detection method of pentaacetyl sucrose. Background technique [0002] Sucralose, chemical name 4,1',6'-trichloro-4,1',6'-trideoxygalactose, is a high-sweetness non-nutritive sweetener with high sweetness and calories The value is 0, acid and alkali resistance, high temperature resistance, safety and non-toxic and other excellent properties. Now it has been widely used in various food and pharmaceutical additives, representing the development direction of strong sweeteners. [0003] [0004] Sucralose was first synthesized by the British Tate & Lyte Company, and was jointly developed and produced by the Johnson Company of the United States after the 1980s. After more than ten years of biochemical and toxicity tests, it was approved by the US Food and Drug Administration (FDA) in 1988. It has be...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 王仲孚黄琳娟邱文龙
Owner NORTHWEST UNIV
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