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Method for detecting polychlorinated biphenyls in seafood

A technology for polychlorinated biphenyls and detection methods, which can be applied to measurement devices, instruments, scientific instruments, etc., can solve the problems of high cost, many interference factors, and long time consumption.

Inactive Publication Date: 2018-10-19
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the problems of high cost, long time consumption and many interference factors in the application of the above-mentioned traditional PCB detection method in seafood, the present invention provides a simple, efficient, high-sensitivity, high-recovery and reproducible marine product. Detection method of polychlorinated biphenyls in products

Method used

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  • Method for detecting polychlorinated biphenyls in seafood
  • Method for detecting polychlorinated biphenyls in seafood
  • Method for detecting polychlorinated biphenyls in seafood

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] Example 1. Detection of polychlorinated biphenyls in small yellow croaker

[0070] Step (1). Sample collection and sample preparation:

[0071] Pack the collected small yellow croakers with clean aluminum foil and seal them in polyethylene bags, then transport them back to the laboratory in a portable refrigerator, remove the scales and skin, and take the muscles along the back. Cut the sample into no more than 0.5cm×0.5cm×0.5cm, homogenize it with a high-speed tissue grinder, dry it in a freeze dryer for 12 hours after homogenization, take it out and store it in a freezer at -18°C until testing;

[0072] Step (2). Sampling and ultrasonic extraction:

[0073] Weigh 4.00g of the small yellow croaker sample to be tested, add 15mL of n-hexane:dichloromethane:acetone (3:1:1, v / v), vortex for 2min, and ultrasonically extract at 35°C with 450W power for 15min; when the sample contains sulfur When the background of the compound interferes, add 2g of copper powder for ultraso...

Embodiment 2

[0105] Determination of 7 kinds of polychlorinated biphenyls in Penaeus vannamei in embodiment 2

[0106] Step (1). Sample collection and sample preparation:

[0107] The collected Penaeus vannamei were packaged with clean aluminum foil and sealed in polyethylene bags, and then transported back to the laboratory in a portable refrigerator, where the heads, shells, and appendages were removed, and the muscles were removed. Cut the sample into no more than 0.5cm×0.5cm×0.5cm, homogenize it with a high-speed tissue masher, dry it in a freeze dryer for 18 hours, take it out and store it in a freezer at -18°C until testing;

[0108] Step (2). Sampling and ultrasonic extraction:

[0109] Weigh 4.00g of the Penaeus vannamei sample to be tested, add 10mL of n-hexane: dichloromethane: acetone (3:1:1, v / v), vortex for 1min, and ultrasonically extract at 35°C with 400W power for 20min; When the background interference of sulfur-containing compounds, add 1g of copper powder for ultrasoni...

Embodiment 3

[0129] Determination of 7 kinds of polychlorinated biphenyls in embodiment 3 razor clams

[0130] Step (1). Sample collection and sample preparation:

[0131] The collected razor clams were packaged with clean aluminum foil and sealed in polyethylene bags, then transported back to the laboratory in a portable refrigerator, shelled, and edible parts were taken. Cut the sample into no more than 0.5cm×0.5cm×0.5cm, homogenize it with a high-speed tissue masher, dry it in a freeze dryer for 24 hours, take it out and store it in a freezer at -18°C until testing;

[0132] Step (2). Sampling and ultrasonic extraction:

[0133] Weigh 4.00g of the razor clam sample to be tested, add 20mL of n-hexane: methylene chloride: acetone (3:1:1, v / v), vortex for 3min, and ultrasonically extract at 40°C for 10min with 500W power; there is sulfur in the sample For the background interference of the compound, add 3g of copper powder for ultrasonic desulfurization, centrifuge at 3000r / m for 5min at...

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Abstract

The invention relates to the technical field of seafood pollution detection, and especially relates to a method for detecting polychlorinated biphenyls in a seafood. The method comprises the followingsteps: (1) sample collection, and sample preparation; (2) sampling and ultrasonic extraction; (3) concentrating, and fat content detection; (4) concentrated sulfuric acid purification, and concentrating; (5) dispersion, solid phase extraction and purification; (6) gas chromatography-electron capture detector detection; (7) standard curve drawing; and (8) detection of the content and the recoveryrate of the polychlorinated biphenyls. The method adopts ultrasonic extraction, dispersion, solid phase extraction and purification, and gas chromatography-electron capture detection technologies to detect the polychlorinated biphenyls in the seafood, has the advantages of simplicity in operation, high efficiency, and flexibility in selection of one-step purification and two-step purification, allows the dispersion, solid phase extraction and purification process to only take 1 min, the result to be accurate, the detection limit of seven polychlorinated biphenyls to be 0.025-0.038 [mu]g / kg, the recovery rate to be 73-110% and the relative standard deviation (n=5) to be 3.3-6.3%, and has a high sensitivity, a satisfactory recovery rate and a satisfactory reproducibility.

Description

technical field [0001] The invention relates to the technical field of seafood pollution detection, in particular to a detection method for polychlorinated biphenyls in seafood. Background technique [0002] As a typical persistent organic pollutant, polychlorinated biphenyls are widely distributed in environmental media such as water, air, soil, sediment, and organisms, and have strong "three-effects" on the human body. Important chemical products such as exchangers, lubricants, insulating media in transformers and capacitors, plasticizers, paraffin wax extenders, adhesives, organic diluents, dust removers, cutting oils, and carbonless copy paper are widely used in electric power, The fields of plastic processing, chemical industry and printing pose a huge threat to human health and the ecological environment. At present, Soxhlet extraction, vibration extraction, accelerated solvent extraction, ultrasonic extraction, stirring bar adsorption extraction, dispersion liquid-li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/062G01N2030/884
Inventor 胡红美李铁军郝青孙秀梅金衍健应忠真郭远明
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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