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Kit for detecting residual amount of 4-hexylresorcinol in aquatic product, and detection method thereof

A technology for hexyl resorcinol and aquatic products, applied in the field of physical and chemical analysis of chemical substances, can solve problems such as many impurities, and achieve the effects of easy evaporation and concentration, good recovery rate and high selectivity

Inactive Publication Date: 2012-07-04
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But there are many deficiencies: for example: 4-hexylresorcinol is easily soluble in ethanol, methanol, glycerol, ether, chloroform, benzene and vegetable oil, and there are too many impurities extracted by methanol and ethanol, especially the highly polar ones Impurities; choose methanol as the extraction solvent after C 18 Column cleanup; therefore, in order to obtain good recovery, it is necessary to select a suitable extraction solvent

Method used

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  • Kit for detecting residual amount of 4-hexylresorcinol in aquatic product, and detection method thereof
  • Kit for detecting residual amount of 4-hexylresorcinol in aquatic product, and detection method thereof
  • Kit for detecting residual amount of 4-hexylresorcinol in aquatic product, and detection method thereof

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Experimental program
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Effect test

Embodiment 1

[0048] Embodiment 1: the detection kit of 4-hexylresorcinol residual amount in the aquatic product of the present invention

[0049] The components of the kit of the invention include a sample extraction solvent and a purification solvent, wherein the extraction solvent is ethyl acetate, and the purification solvent is methanol-acetonitrile-water solution and acetonitrile saturated n-hexane solution. The volume ratio of methanol, acetonitrile and water in the methanol-acetonitrile-water solution is 1:2:1. When using the kit to detect the residual amount of 4-hexylresorcinol, the used volume ratio of the methanol-acetonitrile-water solution to the acetonitrile-saturated n-hexane solution is 1:1.

Embodiment 2

[0050] Embodiment 2: the method for detecting 4-hexylresorcinol residual amount in aquatic product with kit of the present invention

[0051] Detect 4-hexylresorcinol residual amount in aquatic product with test kit of the present invention, carry out as follows:

[0052] (1) Sample extraction: Weigh 2g of the sample (accurate to 0.01g) into a 50mL centrifuge tube, add 20mL of extraction solvent ethyl acetate and 3g of anhydrous sodium sulfate, homogenize for 30s, centrifuge at 4000r / min for 3min, and the supernatant Transfer anhydrous sodium sulfate to the concentrating bottle, take another centrifuge tube, add 15 mL of extraction solvent ethyl acetate to wash the knife head of the homogenizer, transfer the washing liquid into the first centrifuge tube, and extract by vortex shaker for 1 min , centrifuged at 4000r / min for 3min, combined the washing liquid into a 100mL concentrator bottle, and concentrated to dryness by rotary evaporation at 38°C.

[0053](2) Purification: Ad...

Embodiment 3

[0074] Embodiment 3: Comparative experiment of this kit and other kits

[0075] (1) Selection experiment of sample extract

[0076] In this experiment, methanol, acetonitrile and ethyl acetate were used for extraction, and the specific steps were carried out according to Example 2. Experiments show that all of the three have satisfactory recovery rates, but methanol and acetonitrile extract more impurity peaks than ethyl acetate, and the liquid chromatography of shrimp samples extracted by each solvent can be found in Figure 1-3 , figure 1 is the liquid chromatogram of the acetonitrile extraction of the shrimp sample, figure 2 is the liquid chromatogram of methanol extraction of shrimp samples, image 3 is the liquid chromatogram of the ethyl acetate extraction of the shrimp sample; see Table 1 for the recoveries of each solvent extraction. Ethyl acetate has a low boiling point and is easier to evaporate and concentrate, which can shorten the experimental time. Therefore...

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Abstract

The invention provides a kit for detecting the residual amount of 4-hexylresorcinol in an aquatic product. The kit comprises a sample extraction solvent, namely ethyl acetate, and purification solvents, namely a methanol-acetonitrile-aqueous solution and an acetonitrile saturated n-hexane solution, wherein the volume ratio of methanol to acetonitrile to water is 1:2:1; and the volume ratio of the used methanol-acetonitrile-aqueous solution to used the acetonitrile saturated n-hexane solution is 1:1. The invention also provides a method for detecting the residual amount of the 4-hexylresorcinol. The method comprises the following steps of: (1) extracting a sample; (2) purifying; and (3) measuring by virtue of liquid chromatography. According to the kit, ethyl acetate used as the sample extraction solvent has a small number of impurity peaks, and is more easy to evaporate and condense; by utilizing liquid-liquid distributed purification, the recycling rate is higher and the purification effect is better; a liquid chromatography fluorescence detector is used for measurement, and an external standard method is adopted for quantification, so that the effects of high selectivity and high sensitivity can be achieved; and the kit is widely applied to measurement on the residual amount of 4-hexylresorcinol in aquatic products, such as shrimps, fishes, crabs and the like.

Description

technical field [0001] The invention relates to the field of physical and chemical analysis of chemical substances, in particular to a kit for detecting the residual amount of 4-hexylresorcinol in aquatic products and a detection method thereof. Background technique [0002] 4-Hexylresorcinol (4-Hexylresorcinol, 4-HR), alias 2,4-dihydroxyhexylbenzene, hexarasine, 4-HR, CAS number 133-77-6, 4-hexylm-benzene The structural formula of the diphenol drug is as follows: [0003] [0004] 4-Hexylresorcinol is white or yellow-white needle-like crystals with weak odor and strong astringent taste; light brown or pink when exposed to light and air, slightly soluble in water, ethanol, methanol, glycerin, ether, chloroform, Benzene and vegetable oils. 4-Hexylresorcinol is a new type of antioxidant and color-protecting agent that can inhibit browning. Used to keep shrimp, crab and other crustaceous aquatic products in good color and not black during storage (the blackening of shrimp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/12
Inventor 林海丹席静邹志飞谢守新邵琳智陈毓芳林峰
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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