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Method for detecting short-chain chlorinated paraffin in marine products

A technology of short-chain chlorinated paraffin and detection method, which is used in measurement devices, instruments, scientific instruments, etc.

Active Publication Date: 2021-03-19
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims to solve the above-mentioned technical problems existing in the existing short-chain chlorinated paraffin detection method, and provides a method that is simple to operate, does not need to use additional organic solvents in the purification process, is environmentally friendly, has a high degree of automation, is accurate in results, and has a high A method for the detection of short-chain chlorinated paraffins in seafood with good sensitivity and satisfactory recovery and reproducibility

Method used

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  • Method for detecting short-chain chlorinated paraffin in marine products
  • Method for detecting short-chain chlorinated paraffin in marine products
  • Method for detecting short-chain chlorinated paraffin in marine products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) Sampling and sample preparation

[0048] Remove the scales and skin of the small yellow croaker, and take muscle samples along the back. The samples are not larger than 0.5cm×0.5cm×0.5cm.

[0049] (2) Sampling and accelerated solvent extraction

[0050] Weigh four samples to be tested, each 2.00g, perform four accelerated solvent extractions on the samples to be tested and collect the extracts. The specific steps for accelerated solvent extraction are: fill the bottom of the 34mL extraction pool with 3g of activated florisil Earth, 5g of activated neutral silica gel and 1g of activated anhydrous sodium sulfate; mix the sample to be tested with an appropriate amount of diatomaceous earth and put it into the extraction cell, add 1ng to replace the internal standard 13 C10-trans chlordane, the top of the pool of the extraction tank is filled with an appropriate amount of diatomaceous earth; with the volume ratio (v / v) of 1:1, normal hexane and dichloromethane are used...

Embodiment 2

[0075] (1) Sampling and sample preparation

[0076] Remove the head, shell, and appendages of Portunus trituberculatus, and take muscle samples. The samples are not larger than 0.5cm×0.5cm×0.5cm. After mashing and homogenizing, dry in a freeze dryer for 24 hours, and refrigerate at -80°C , to be tested.

[0077] (2) Sampling and accelerated solvent extraction

[0078] Weigh four parts of samples to be tested, each 2.00g, carry out accelerated solvent extraction on the samples to be tested respectively and collect the extract. The specific steps of accelerated solvent extraction are: fill 5g of activated florisil at the bottom of the 34mL extraction pool, 3g of activated neutral silica gel and 1g of activated anhydrous sodium sulfate; mix the sample to be tested with an appropriate amount of diatomaceous earth and put it into the extraction cell, add 1ng to replace the internal standard 13 C10-trans chlordane, the top of the pool of the extraction tank is filled with an appro...

Embodiment 3

[0092] (1) Sampling and sample preparation

[0093] Remove the shell of the razor clam and take a sample of the edible part. The sample is not larger than 0.5cm×0.5cm×0.5cm. After mashing and homogenizing, dry it in a freeze dryer for 18 hours and refrigerate at -80°C until testing.

[0094] (2) Sampling and accelerated solvent extraction

[0095] Weigh four parts of samples to be tested, each 2.00g, carry out accelerated solvent extraction on the samples to be tested respectively and collect the extract. The specific steps of accelerated solvent extraction are: fill 4g of activated florisil at the bottom of the 34mL extraction pool, Activated 4g neutral silica gel and activated 1g anhydrous sodium sulfate; mix the sample to be tested with an appropriate amount of diatomaceous earth and put it into the extraction cell, add 1ng to replace the internal standard 13 C10-trans chlordane, the top of the pool of the extraction tank is filled with an appropriate amount of diatomaceou...

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Abstract

The invention discloses a method for detecting short-chain chlorinated paraffin in marine products. The method comprises the following steps of: (1) sampling and sample preparation; (2) sampling and accelerated solvent extraction; (3) degreasing and impurity removal; (4) headspace solid phase microextraction; (5) gas chromatography-mass spectrometry detection; (6) standard curve drawing; and (7) sample determination. According to the method, the sample purification treatment process and detection conditions are optimized; the accelerated solvent extraction, headspace solid-phase microextraction and gas chromatography-mass spectrometry are adopted to determine the short-chain chlorinated paraffin in the marine products, and therefore, the method is simple to operate, does not need an additional organic solvent in the purification process, is environment-friendly, meets the requirements of green development, and is suitable for large-scale popularization and application; The whole accelerated solvent extraction and headspace solid-phase microextraction processes can be completed through instruments, and therefore, the method has the advantages of high automation degree, accurate result, high sensitivity, satisfactory recovery rate and reproducibility, and the method can be used for measuring the content of the short-chain chlorinated paraffin in the marine products.

Description

technical field [0001] The invention relates to the technical field of seafood pollution detection, in particular to a method for detecting short-chain chlorinated paraffins in seafood. Background technique [0002] Short-chain chlorinated paraffins, polychlorinated n-alkanes with a carbon chain length of C 10 -C 13 (chlorine content is 30%-70%), since the 1930s, it has been widely used in metalworking fluids, flame retardants, plasticizers, paints, leather and sealants and other fields. Evidence that SCCPs have been detected in all biospheres, including human tissues, is of great concern to the scientific community. Due to its chemical stability and high toxicity, it can bioaccumulate and biomagnify through the food web. Once it is eaten by humans, it will pose adverse risks to human health. It has been included in the "Stockholm Convention" to limit short-chain chlorinated paraffins in other chlorine. Presence in paraffin mixtures. Seafood is an important part of the s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N2030/062G01N2030/045
Inventor 胡红美郭远明李铁军应忠真孙秀梅
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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