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Rapid extraction, purification and detection method of Sudan red dye residue in food

A detection method and technology for Sudan red, applied in the field of rapid extraction, purification and detection of Sudan red dye residues, can solve the problems of low sensitivity, large matrix interference, single sample matrix, etc., to overcome poor sensitivity, omit sample extraction steps, operation handy effect

Inactive Publication Date: 2016-11-09
NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Similarly, the high-performance liquid chromatography-ultraviolet detector used in this method has defects such as low sensitivity and high false positive rate. At the same time, the sample matrix is ​​single, and the egg samples and chili oil samples that are of public concern are not involved, and the method has not been tested. Purification and direct measurement, large matrix interference

Method used

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  • Rapid extraction, purification and detection method of Sudan red dye residue in food
  • Rapid extraction, purification and detection method of Sudan red dye residue in food
  • Rapid extraction, purification and detection method of Sudan red dye residue in food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1.1 Dried fresh peppers and crushed to obtain pepper powder, then weighed 1.0g of pepper powder into a 50mL plastic centrifuge tube, added 5mL of acetonitrile-dichloromethane mixture with a volume ratio of 1:0.5, ultrasonically extracted for 1min, centrifuged for 5min, and repeated Extracted twice, combined extracts, concentrated by rotary evaporation to near dryness to obtain extracts, redissolved extracts with 2mL n-hexane, purified through solid-phase extraction cartridges, collected eluents in 10mL glass centrifuge tubes, blown to dryness with nitrogen , adding 1 mL of tert-butyl methyl ether-methanol mixed solution with a volume fraction of 10% tert-butyl methyl ether to redissolve, and passing through a 0.22 μm filter membrane to obtain a purified solution for testing.

[0037] 1.2 The purification solution of the capsicum sample that step 1.1 obtains is carried out ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS / MS analysis) analysis according t...

Embodiment 2

[0044] 2.1 Dry and pulverize the dried chilies to obtain chili powder, then weigh 2.0g of chili powder into a 50mL plastic centrifuge tube, add 10mL of acetonitrile-dichloromethane mixture with a volume ratio of 1:1, ultrasonically extract for 5min, and centrifuge for 5min , repeated the extraction twice, combined the extracts, concentrated by rotary evaporation until nearly dry to obtain the extract, redissolved the extract with 5mL of n-hexane, purified it through a solid phase extraction column, collected the eluate in a 10mL glass centrifuge tube, blown with nitrogen To dryness, add 1 mL of tert-butyl methyl ether-methanol mixed solution with a volume fraction of 40% tert-butyl methyl ether to redissolve, and pass through a 0.22 μm filter membrane to obtain a purified solution for testing.

[0045] 2.2 The purified solution of the pepper sample obtained in step 2.1 was subjected to UFLC-MS / MS analysis according to the conditions of Example 1. Unlike Example 1, the concentra...

Embodiment 3

[0047] 3.1 Further dry and crush the chili powder to obtain chili powder, weigh 4.0g of chili powder into a 50mL plastic centrifuge tube, add 10mL of acetonitrile-dichloromethane mixture with a volume ratio of 1:5, ultrasonically extract for 8min, centrifuge for 5min, repeat Extracted twice, combined extracts, concentrated by rotary evaporation until nearly dry to obtain extracts, redissolved extracts with 8mL n-hexane, purified through solid phase extraction cartridges, collected eluents in 10mL glass centrifuge tubes, blown to dryness with nitrogen , adding 1 mL of tert-butyl methyl ether-methanol mixed solution with a volume fraction of 50% tert-butyl methyl ether to redissolve, and passing through a 0.22 μm filter membrane to obtain a purified solution for testing.

[0048] 3.2 The purified solution of the pepper sample obtained in step 3.1 was subjected to UFLC-MS / MS analysis according to the conditions of Example 1. Unlike Example 1, the concentration of formic acid in mo...

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Abstract

The invention relates to a fast extraction, purification and detection method for Sudan red dye residues in food. The food is one of eggs, chilies and chili oil. The method comprises the following steps: an egg sample or a chili sample is extracted with acetonitrile-dichloromethane mixed liquor and then purified with a strong cation solid-phase extraction column, while a chili oil sample is mixed with dichloromethane-n-hexane and directly purified with the column; and detection is performed with UFLC-MS / MS (ultrafast liquid chromatography tandem mass spectrometry). The method overcomes the defect of low recovery rate of Sudan red III and Sudan red IV, solves the problems that the egg sample is dispersed easily and effective solid-liquid separation cannot be realized easily, and has the advantages of simple steps and convenience in operation; meanwhile, purified liquor after treatment is subjected to Sudan red content detection with the UFLC-MS / MS, the defects of poor sensitivity, low accuracy, high false positive rate and the like of the conventional liquid chromatography are overcome, the recovery of standard addition of four Sudan red dyes is 90.6%-99.4%, and the detection limit is 0.1-0.5 mu g / kg.

Description

technical field [0001] The invention relates to a method for determining the residue of toxic and harmful chemical components in food, in particular to a method for rapid extraction, purification and detection of Sudan red dye residue in foods such as eggs and peppers. Background technique [0002] Sudan red is a kind of synthetic azophenyl naphthol industrial dyes, mainly including four types I, II, III and IV, which are widely used in industrial products such as engine oil, gasoline wax and shoe polish, and can also be used in fireworks Coloring of fireworks. In the process of food processing, in order to improve the sensory properties of food and increase people's appetite, some food coloring is often added in order to make the color of the product bright or maintain the original color. In 1995, the European Union prohibited adding Sudan Red (especially Sudan Red No. 1) to food as a food coloring, and my country also expressly prohibited it. However, in recent years, Su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/14G01N30/02
Inventor 陈晓红潘胜东赵永纲金米聪
Owner NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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