Pretreatment technology for detecting polybrominated diphenyl ethers residue in vegetables

A polybrominated diphenyl ether and vegetable technology, which is applied in the field of analytical chemistry, can solve the problems of large consumption of organic solvents, complicated purification process and high detection cost, and achieves the effects of less organic solvent consumption, high extraction efficiency and less environmental pollution

Inactive Publication Date: 2017-03-22
INST OF SOIL SCI CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the problems of large solvent consumption, incomplete extraction, long time-consuming, complicated and incomplete purification process in the existing vegetable pretreatment technology, the present invention provides a pretreatment technology for the detection of polybrominated diphenyl ether residues in vegetables, using accelerated solvent extraction The technology extracts PBDEs residu...

Method used

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  • Pretreatment technology for detecting polybrominated diphenyl ethers residue in vegetables
  • Pretreatment technology for detecting polybrominated diphenyl ethers residue in vegetables
  • Pretreatment technology for detecting polybrominated diphenyl ethers residue in vegetables

Examples

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Embodiment 1

[0038] This embodiment focuses on the GC-ECD analysis of polybrominated diphenyl ethers (PBDEs) in the standard solution to ensure the qualitative and quantitative accuracy of PBDEs.

[0039] Step 1: Take 500 μL of the above 10 kinds of PBDEs mixed standard stock solution in a 2 mL injection bottle, add 500 μL of n-hexane to dilute to 500 μg L -1 , and then serially diluted to 250 μg L in new vials -1 , 100μg L -1 , 50μgL -1 , 25 μg L -1 , 10 μg L -1 , 5 μg L -1 , detected using GC-ECD.

[0040] Step 2: Set the chromatographic condition parameters: the chromatographic column is a DB-5 column (30m×0.32mm×0.25μm), the temperature of the injection port is 265°C, the carrier gas is nitrogen, the flow rate is 2mL / min, and the detector temperature is 298 ℃, the injection volume was 1 μL, splitless injection.

[0041] Step 3: Set the heating program: the initial temperature is 140°C, keep for 2min, rise to 180°C at 5°C / min, keep for 5 minutes; rise to 265°C at 5°C / min, keep fo...

Embodiment 2

[0048] This example focuses on the accelerated solvent extraction (ASE) of 10 kinds of PBDEs in vegetables, and optimizes the extraction conditions of ASE.

[0049] Step 1. Wash the surface of the vegetable sample with deionized water, dry the surface moisture under natural conditions, cut into pieces of about 0.5cm with scissors, accurately weigh the sample in a mortar, add 50μL 100μg L -1 The mixed standard solution of 10 kinds of PBDEs was added with 1g of quartz sand and 2g of diatomaceous earth, fully ground and transferred to the ASE stainless steel extraction pool, and extracted by ASE 200 accelerated solvent extraction (DIONEX, USA). Using n-hexane: acetone (4:1, v / v) for extraction, the furnace temperature of the extraction pool is 100°C, and the pressure is 1500Psi. Extraction process: heating for 5 minutes, static extraction for 5 minutes to flush 60% of the volume, nitrogen purging for 60 seconds, and cycle 2 times.

[0050] Step 2. Use n-hexane: dichloromethane ...

Embodiment 3

[0059] This example focuses on the preparation process of the self-prepared SPE purification column and its elution behavior of PBDEs.

[0060] Step 1. Select two kinds of fillers commonly used in the laboratory, silica gel and florisil. The treatment steps of the two fillers are as follows: (1) Deactivation: the filler is placed in an evaporating dish, and baked in an oven at 200 ° C for 12 hours , transferred to a desiccator, cooled to room temperature, and set aside; (2) Activation: The filler needs to be activated before use: take an appropriate amount of filler, add 5% (mass ratio) deionized water, mix well, and place on a shaker to vibrate and mix. Mix well until there are no lumps in the filling, and equilibrate overnight. Acidic silica gel was prepared by modification with concentrated sulfuric acid. The specific steps are as follows: Weigh the filler and place it in a flask, add concentrated sulfuric acid drop by drop according to filler: concentrated sulfuric acid 5:...

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Abstract

The invention discloses pretreatment technology for detecting polybrominated diphenyl ethers residue in vegetables and belongs to the technical field of analytical chemistry. The pretreatment technology includes steps: 1, performing ASE extraction on a ground vegetable sample; concentrating extract; 3, loading a sample of the concentrated extract to an activated florisil-acidic silica gel solid-phase extraction purifying column, and using normal hexane for elution; 4, blow-drying eluent, and adding a fixed amount of normal hexane for re-dissolving; 5, performing gas chromatography-electronic capture device (GC-ECD) detection. The pretreatment technology has the advantages of simple operation, high speed and high extraction efficiency. The solid-phase extraction purifying column which is self-prepared is adopted to purify vegetable extract, so that purifying effect is good and cost is low. GC-ECD detection finds that the pretreatment technology is efficient and sensitive and is high in efficiency in extracting the PBDEs in the vegetables, good in purifying effect and suitable for pretreatment of qualitative and quantitative analysis of the PBDEs residue in the vegetables.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and more specifically relates to a pretreatment technology for detecting polybrominated diphenyl ether residues in vegetables. Background technique [0002] As a class of brominated flame retardants (BFRs), polybrominated diphenyl ethers (Polybrominated diphenyl ethers, referred to as PBDEs) have the advantages of high flame retardant efficiency, good thermal stability, and low price, and are often added to polymers such as polystyrene and polyurethane foam. Synthetic materials, and widely used in industrial products such as electronic products, textiles, building materials and furniture. PBDEs belong to persistent organic pollutants (POPs), which are hydrophobic, persistent and bioaccumulative, and are easy to adsorb in particulate matter and sediments and enrich in organisms, and can migrate long distances in the environment. PBDEs are difficult to degrade in the environment and h...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/14
CPCG01N30/06G01N30/14G01N2030/062
Inventor 王芳相雷雷卞永荣蒋新谷成刚杨兴伦宋洋叶茂
Owner INST OF SOIL SCI CHINESE ACAD OF SCI
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