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Method for improving detection precision of polychlorinated biphenyl in wholphin fat and application thereof

A polychlorinated biphenyl and detection accuracy technology, applied in the field of marine pollution detection, can solve the problems of many interference factors and low efficiency, and achieve the effects of high precision and sensitivity, low improvement efficiency, good recovery rate and reproducibility

Active Publication Date: 2021-03-05
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the above-mentioned deficiencies in the prior art, the present invention proposes a method for improving the detection accuracy of PCBs in cetacean fat, thereby improving the problems of low efficiency and many interference factors in the detection of PCBs in cetacean fat , making the detection method simple and efficient, with high precision and sensitivity, good recovery and reproducibility

Method used

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  • Method for improving detection precision of polychlorinated biphenyl in wholphin fat and application thereof
  • Method for improving detection precision of polychlorinated biphenyl in wholphin fat and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1 A method for improving the detection accuracy of polychlorinated biphenyls in cetacean fat

[0034] Prior to the detection of PCBs in cetacean fat samples, the following sample pretreatments were performed:

[0035] (1) Sampling: After the cetacean (Chinese white dolphin) fat sample is thawed, take about 0.3g into a mortar, add 2g of anhydrous sodium sulfate to fully grind, transfer to a filter paper tube, add 5ng 13C-PCB141 marker recovery indicator ( 13 C-PCB141 is similar to the PCBs measured in this embodiment, and is used to characterize the loss or recovery rate of the entire pretreatment process).

[0036] (2) Extraction: Add 200mL of dichloromethane (DCM) / n-hexane (HEX) mixed solvent [DCM:HEX=3:1 (V / V)] into the flask, and perform Soxhlet extraction for 48h.

[0037] (3) Solvent conversion: Rotate the extract obtained in step (2) to about 1mL, transfer it to a graduated glass centrifuge tube, dilute to 10mL with n-hexane, and concentrate to 2mL. ...

Embodiment 2

[0043] Embodiment 2 A method for improving the detection accuracy of polychlorinated biphenyls in cetacean fat

[0044] Prior to the detection of PCBs in cetacean fat samples, the following sample pretreatments were performed:

[0045] (1) Sampling: After the cetacean (Chinese white dolphin) fat sample is thawed, take about 0.2g into a mortar, add 2g of anhydrous sodium sulfate to fully grind, transfer to a filter paper tube, add 5ng 13 C-PCB141 labeled recovery indicator.

[0046] (2) Extraction: Add 200mL of dichloromethane (DCM) / n-hexane (HEX) mixed solvent [DCM:HEX=2:1 (V / V)] into the flask, and perform Soxhlet extraction for 50h.

[0047] (3) Solvent conversion: Rotate the extract obtained in step (2) to about 0.5 mL, transfer it to a graduated glass centrifuge tube, use n-hexane to set the volume to 8 mL, and concentrate to 1 mL. Gel chromatography column (GPC).

[0048] (4) GPC column: the column specification is 50cm×2.5cm i.d. glass column, and the piston is made o...

Embodiment 3

[0053] Embodiment 3 A method for improving the detection accuracy of polychlorinated biphenyls in cetacean fat

[0054] Prior to the detection of PCBs in cetacean fat samples, the following sample pretreatments were performed:

[0055] (1) Sampling: After the cetacean (Chinese white dolphin) fat sample is thawed, take about 0.3g into a mortar, add 2g of anhydrous sodium sulfate to fully grind, transfer to a filter paper tube, add 5ng 13 C-PCB141 labeled recovery indicator.

[0056] (2) Extraction: add 150mL dichloromethane (DCM) / n-hexane (HEX) mixed solvent [DCM:HEX=4:1 (V / V)] into the flask, and perform Soxhlet extraction for 50h.

[0057] (3) Solvent conversion: Rotate the extract obtained in step (2) to about 1.5mL, transfer it to a graduated glass centrifuge tube, dilute to 12mL with n-hexane, and concentrate to 3mL. Gel chromatography column (GPC).

[0058] (4) GPC column: the column specification is 50cm×2.5cm i.d. glass column, and the piston is made of polytetrafluo...

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Abstract

The invention belongs to the technical field of marine pollution detection, and particularly relates to a method for improving detection precision of polychlorinated biphenyl in wholphin fat and an application of the method. The method comprises the following steps: before the polychlorinated biphenyl in a wholphin fat sample is detected, carrying out Soxhlet extraction on the wholphin fat sampleby using a dichloromethane / normal hexane mixed solvent; and concentrating an extracting solution with n-hexane in a constant volume manner, sequentially eluting with a GPC column and an acidic silicagel column to finally obtain a to-be-detected target compound, and detecting polychlorinated biphenyl in wholphin fat by adopting the to-be-detected target compound obtained by the method through an existing polychlorinated biphenyl detection method. The method can effectively improve the problems of low efficiency and many interference factors in the detection of polychlorinated biphenyl in wholphin fat, and has the advantages of simplicity, high efficiency, high precision and sensitivity, and good recovery rate and reproducibility.

Description

technical field [0001] The invention belongs to the technical field of marine pollution detection, and in particular relates to a method for improving the detection accuracy of polychlorinated biphenyls in cetacean fat and an application thereof. Background technique [0002] Polychlorinated biphenyls (PCBs) are typical persistent organic pollutants, which are widely distributed in environmental media such as water, air, soil, sediment, and organisms, and have strong "three-effects" on the human body. ", have been used as important chemical products such as heat exchangers, lubricants, insulating media in transformers and capacitors, plasticizers, paraffin wax extenders, adhesives, organic diluents, dust removers, cutting oils, and carbonless copy paper , Widely used in fields such as electric power, plastic processing, chemical industry and printing, poses a huge threat to human health and the ecological environment. At present, Soxhlet extraction, vibration extraction, ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/60
CPCG01N30/02G01N30/06G01N30/14G01N30/60G01N2030/062
Inventor 谢强吴玉萍郭永卫
Owner SUN YAT SEN UNIV
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