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Sudan red I crystal A and preparation method thereof

A technology of Sudan red and crystal, applied in the new crystalline form crystal A of Sudan red I and the field of preparation thereof, can solve the problems of far difference, low content of Sudan red I, unable to meet the requirements of standard substances, etc., and achieve good particle uniformity. degree of effect

Inactive Publication Date: 2015-01-07
NAT INST OF METROLOGY CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content and purity of Sudan Red I prepared by this method are often low, usually only 60-80%, and can be used as a dyestuff, but it is far from the requirement that the standard substance content is higher than 99%.
[0006] In food hygiene testing, if you want to determine the content of Sudan Red I in a food sample, you need to have a known content of Sudan Red I standard substance as an external standard for comparison, and the experimental method of sample pretreatment also needs to use a known and accurate content. The reference substance was used for the sample recovery experiment, and the content of Sudan I prepared by the prior art was too low to meet the requirements as a standard substance.

Method used

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  • Sudan red I crystal A and preparation method thereof
  • Sudan red I crystal A and preparation method thereof
  • Sudan red I crystal A and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Example 1 Preparation of Sudan Red I Crystal A

[0063] Take Sudan Red I (Acros Company, reagent grade, purity > 95%) micropowder solid 120g, put in a 2000ml spherical three-necked flask, add toluene (Beijing Chemical Reagent Company, analytical grade) 1450ml, add purified water 300ml, install a stirring device, spherical Reflux condenser. Adjust the rotation speed at 100-200r / min and stir slowly with a water bath (60°C) until it is completely dissolved, keep stirring (rotation speed 200rpm) for half an hour and then stop heating. Leave to stand for stratification, remove the lower aqueous phase with a separatory funnel, add 10 g of activated carbon (source: Beijing Dali Fine Chemical Factory, specification: analytical pure) to the organic phase, continue heating and stirring for 1 hour to decolorize, and use a medium-speed chemical analysis filter paper (Hangzhou Fuyang Special Paper Co., Ltd.) to filter while hot (filter paper source and specifications), remove activ...

Embodiment 2

[0065] The content determination and calibration of the standard substance of embodiment 2 Sudan Red I

[0066] Use high performance liquid chromatography to measure the crystal A purity of the Sudan red I prepared by embodiment 1

[0067] Mobile phase: Phase A: 20mM ammonium acetate solution

[0068] Phase B: Methanol

[0069] Gradient elution program: (0-5) min, 50% B; (5-15) min, 100% B; (15-25) min, 100% B;

[0070] Flow rate: 1.1mL / min;

[0071] Injection volume: 10μl injection;

[0072] The sample is 1000 μg / mL Sudan Red I methanol solution.

[0073] Detection wavelength: 230nm / 478nm

[0074] Chromatographic column: Inertsil ODS-SP, 250mm×4.6×5μm

[0075] Sample: Prepare the solution of Sudan Red Ⅰ, inject 2-3 times for each sample. Blank samples were injected 2 times.

[0076] The liquid chromatographic test results of Sudan Red Ⅰ standard substance are shown in Table 1:

[0077] Table 1 Liquid Chromatography Test Results of Sudan Red Standard Substance...

Embodiment 3

[0079] The homogeneity check of the standard substance of embodiment 3 Sudan Red I

[0080] Take 5 parts of samples from different parts of the Sudan I crystal A prepared in Example 1, add water to make a 1mg / mL solution, randomly select 15 packages from each standard substance, and carry out the uniformity test between the bottle and the bottle , the test method is the HPLC method of the fixed value method, the test results in the bottle and between the bottles are carried out statistical calculations with statistical methods (F test), to judge its uniformity, the test results are shown in Table 2. As can be seen from the test results, the pure Sudan I prepared in Example 1 has good uniformity.

[0081] Table 2 The homogeneity test results of Sudan red standard substance

[0082]

[0083]

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Abstract

The invention relates to Sudan red I crystal A. Crystal Sudan red I exists in a polymorphic form with a main crystal form and other multiple auxiliary crystal forms, and the polymorphic form is identified through X-ray powder diffraction. The invention further provides a preparation method of the Sudan red I crystal A; the purity of the Sudan red I crystal A is greatly improved, the content of the Sudan red I crystal A is greatly increased, a prepared sample meets the technical index for detection of Sudan red I in a food as an external marker, and a special Sudan red I standard substance for food detection is further prepared.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a new crystal form crystal A of Sudan red I and a preparation method thereof. Background technique [0002] The chemical name of Sudan I (Sudan I) is 1-phenylazo-2-naphthalenol (1-phenylazo-2-naphthalenol), and its molecular structure is C 16 h 12 ON 2 , molecular weight 248.28. [0003] Sudan Red I is a synthetic industrial dye, which is commonly used in industry, such as the dyeing of solvents, motor oil, wax and shoe polish. Its use in food production is banned in most countries around the world. The International Agency for Research on Cancer (IARC) classifies Sudan Red I as a three-category carcinogen, that is, animal carcinogens, mainly based on the research results of in vitro and animal experiments, and Sudan Red I has sensitization and can be Cause human dermatitis. Toxicology research experiments have shown that Sudan Red No. 1 can cause cancer in mi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C245/10G01N30/02
Inventor 马康张伟
Owner NAT INST OF METROLOGY CHINA
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