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Liquid chromatography-mass spectrometry detection method for detecting acid azo colorants in animal dried aquatic products

A liquid-mass spectrometry, detection method technology, applied in measuring devices, instruments, scientific instruments, etc., to achieve high recovery rate, ensure parallelism, and improve recovery rate

Active Publication Date: 2020-01-17
江苏省食品药品监督检验研究院
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Problems solved by technology

Xu Xueqin and others invented a method for the determination of Acid Scarlet GR in paper food packaging materials. The sample was ultrasonically extracted with methanolic acetic acid aqueous solution, and the sample was filtered directly into ultra-high performance liquid chromatography-quadrupole mass spectrometry (UPLC-MS). Determination, but this pretreatment method is not suitable for the matrix with high protein content such as dried aquatic products of animal origin

Method used

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  • Liquid chromatography-mass spectrometry detection method for detecting acid azo colorants in animal dried aquatic products
  • Liquid chromatography-mass spectrometry detection method for detecting acid azo colorants in animal dried aquatic products
  • Liquid chromatography-mass spectrometry detection method for detecting acid azo colorants in animal dried aquatic products

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1 degreasing treatment

[0039] The dried aquatic product samples of animal origin were degreased three times with petroleum ether. Because the 9 kinds of acidic azo colorants are water-soluble azo dyes, oil-containing food is easy to form a water-in-oil structure when adding a water-soluble extract, which affects the extraction rate of the sample; at the same time, degreasing is also a preliminary purification of the sample, which can effectively Avoid clogging and overloading of SPE cleanup cartridges. Therefore, for oil-containing samples, degreasing treatment must be carried out.

[0040] The specific operation is: after the dried shrimp sample is crushed evenly, accurately weigh 2.000g (accurate to 0.001g) of the sample in a 50ml centrifuge tube, add 10ml petroleum ether to the centrifuge tube to remove fat, and vortex for 2 minutes , centrifuge at 8000rpm for 5min, and discard the petroleum ether. Repeat the above steps 3 times to dry the petroleum e...

Embodiment 2

[0041] Embodiment 2 extraction solvent selection and verification

[0042] When extracting, first use alkaline solution ethanol-ammonia-water [(7:2:1) volume ratio] for extraction, and then adjust the solution to be purified to acidity. Selection and validation of extraction solvents. Taking Acid Scarlet GR as an example, 5 different solvents were selected for extraction. The specific operation was as follows: group the samples obtained from degreasing treatment in Example 1, take 5 groups, add 5 kinds of alkaline solutions to the samples obtained from degreasing treatment in each group, and ultrasonically Extract for 5 minutes, centrifuge at 8000rpm for 5 minutes, and take the supernatant; repeat the above steps twice, and combine the extracts. The results are shown in Table 1. It can be seen that the extraction effect of ethanol-ammonia-water [(7:2:1) volume ratio] is the best .

[0043] The reason is that the protein in food is composed of amino acids, and each amino acid...

Embodiment 3

[0046] The concentrated volume verification of embodiment 3 extract

[0047] The specific operation is: add 10 mL of ethanol-ammonia water-water solution (volume ratio 7:2:1) to the sample obtained from degreasing treatment in Example 1, ultrasonically extract for 5 minutes, centrifuge at 8000 rpm for 5 minutes, and take the supernatant. Add 10 mL of ethanol-ammonia water-water solution (volume ratio 7:2:1) to the precipitate to extract again, repeat the above steps twice, combine the supernatant, which is the extract, blow away the ethanol and ammonia at 60°C with nitrogen, and concentrate to below 5mL. Taking Acid Scarlet GR as an example, the concentrated volume of the extract was verified, and the verification results are shown in Table 2.

[0048] Table 2 The effect of the concentrated volume of the extract on the recovery rate of Acid Scarlet GR in dried aquatic products of animal origin

[0049]

[0050] As can be seen from the data in the table, the recovery rate ...

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Abstract

The invention provides a liquid chromatography-mass spectrometry detection method for detecting nine acid azo colorants in animal dried aquatic products. The method comprises the following steps: carrying out homogenization, degreasing and extraction on an animal dried aquatic product sample; carrying out purification with a polyamide solid phase extraction column; and finally carrying out quantitative detection with a liquid chromatography-tandem quadrupole mass spectrometer. A C<18> chromatographic column is used for carrying out gradient elution with methanol and a 10mM ammonium acetate solution. A good linear range, satisfactory recovery and reproducibility are achieved for all the nine colorants. Moreover, the detection limit of the method is up to 0.1 to 1[mu]g / kg, and the quantitative limit is up to 0.25 to 25[mu]g / kg. The method has the advantages of easiness, convenience, rapidness, high recovery and high sensitivity, and is suitable for the detection of nine acid azo colorants in the animal dried aquatic products.

Description

technical field [0001] The invention belongs to the technical field of food safety detection, and relates to a method for measuring acidic azo colorants in dry aquatic products of animal origin by using a liquid mass spectrometer. Background technique [0002] Acidic azo colorants contain azo structure, sulfonic acid groups and phenolic hydroxyl groups in their molecular structure, have strong hydrophilicity and good coloring effect, and are widely used in food processing and industrial production. Among the 9 red and yellow colorants selected in this study, Acid Scarlet GR is a non-edible substance, and there is no standard detection method stipulated by the state at present. Acid Orange II is a non-edible substance regulated by the Ministry of Health, and the remaining 7 colorants can be used as food additives It is used in food processing, but according to the provisions of GB2760-2014 "National Food Safety Standard Food Additives Use Standard", this type of coloring agen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/047G01N2030/062
Inventor 颜春荣高惠敏林慧徐春祥张征
Owner 江苏省食品药品监督检验研究院
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