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Method for synchronously purifying and separating organic extract of environmental medium step by step

A technology of environmental media and extracts, applied in the direction of material separation, analysis materials, measuring devices, etc., can solve the problems of differences in total extract components, incomparability, etc.

Active Publication Date: 2010-05-12
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Different extractants are used for the extraction of organic matter in different existing media, which will lead to differences in the total extract components and are not comparable. The purpose of the present invention is to provide synchronous purification and step-by-step separation of organic extracts in environmental media. method, a systematic method that integrates enrichment, purification, and separation of organic substances in different media, which can be combined with one or several types of toxic effects of organic extracts to determine the characteristics of pollutants that cause the effect

Method used

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  • Method for synchronously purifying and separating organic extract of environmental medium step by step
  • Method for synchronously purifying and separating organic extract of environmental medium step by step
  • Method for synchronously purifying and separating organic extract of environmental medium step by step

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026]Accurately prepare 2L of simulated water samples containing certain concentrations of organic pollutants of different polarities (which contains 8 kinds of organochlorine pesticides (α-HCH, β-HCH, γ-HCH, δ-HCH, p , p'DDE, o, p'-DDT, p, p'-DDD, p, p'-DDT, the concentration is 20ng / L), 28 kinds of polychlorinated biphenyls (CB-8, CB-18, CB -28, CB-52, CB-44, CB-66, CB-81, CB-77, CB-101, CB-123, CB-118, CB-114, CB-105, CB-126, CB-153 , CB-138, CB-128, CB-167, CB-156, CB-157, CB-169, CB-187, CB-180, CB-170, CB-189, CB-195, CB-206, CB -209, the concentration is 20ng / L), 16 polycyclic aromatic hydrocarbons (naphthalene, acenaphthylene, acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene, chrysene, benzo[b]fluorene Anthracene, benzo[k]fluoranthene, benzo[a]pyrene, indeno[1,2,3-c,d]pyrene, dibenzo(a,n)anthracene, and perylene are all 20ng in concentration / L), and nonylphenol (200ng / L), octylphenol (200ng / L), bisphenol A (200ng / L), 17-β...

Embodiment 2

[0041] The method in Example 1 was used to configure, filter and enrich the water samples. The dried HLB column was eluted successively with 10mL n-hexane, 10mL n-hexane / dichloromethane (4:1) and 12mL methanol / dichloromethane (1:1) (flow rate 2mL / min), methanol / dichloromethane After 6 mL of the eluate was collected every 2 mL, it was concentrated to 0.1 mL in a gentle nitrogen flow, and analyzed by HPLC (DVD / FLD), the analysis conditions were as follows: - HPLC (DVD / FLD):

[0042] Mobile phase: 0-5min, methanol: water 80%: 20%; 5-11min, methanol 100%; flow rate: 1ml / min;

[0043] Column temperature: 30°C.

[0044] Detector:

[0045] BPA: FLD detector, λEx = 228nm;

[0046] E2: FLD detector, λEx = 224nm;

[0047] OP, NP: FLD detector, λEx = 226 nm.

[0048] The analysis results showed that when 10 mL of methanol / dichloromethane (4:1) was selected, the recovery rate of NP, OP, BPA, and E2 reached 90% to 110%, and the recovery rate did not increase significantly when the vol...

Embodiment 3

[0050] Put the bottom mud (soil and biological samples) in a refrigerator at -20°C to freeze, and then use a freeze dryer to remove water. After grinding, pass through a 200-mesh sieve and store in a refrigerator at 4°C. Take the ground mud (soil and biological samples) Sample) 20g sample was extracted three times with n-hexane, dichloromethane and methanol Soxhlet respectively (20 hours / time), and 1mL standard sample was added to the extracted soil (in which the concentration of OCs was 50ppb, PCBs was 50ppb, PAHs was 50ppb, phenolic compound is 50ppb), mixed thoroughly as a simulated sediment sample. Respectively with n-hexane / dichloromethane (1:1), n-hexane / dichloromethane (2:1) and n-hexane / dichloromethane ( 4:1) solvent as the extractant to extract the organic matter in the simulated sediment sample. After extraction, it is concentrated to 1mL to measure the concentration. The analysis conditions are as in Example 1 and Example 2. The results show that n-hexane / dichloromet...

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Abstract

The invention discloses a method for synchronously purifying and separating the organic extract of an environmental medium step by step, which belongs to the field of environmental analysis. The method comprises the following steps of: storing suspended substances of a water sample passing through a filter membrane; freeze drying a solid sample, and then grinding or crushing and sieving to obtain a solid-phase sample; enriching the filtered water sample and extracting; and then vacuum drying; eluding solid-phase extraction column with an organic solvent; concentrating eluding liquid; carrying out SoxHlet extraction on a sieved solid-phase sample of a non-organism sample; concentrating the extract liquid and fixing the volume; enriching an organism sample with an organic extract; and then removing macromolecular organisms and pigment with GPC; and finally enriching; drying with florisil, adding the sample solution concentrated in the steps (2) to a florisil column for separating; continuously eluting with the organic solvent; collecting and concentrating eluting liquid respectively used for chemical analysis and toxicity test. The invention applies extraction and separation methods based on the same principle to different environmental media, and can effectively conduct comparison of toxicity and concentration on organic extract of a mixing system.

Description

technical field [0001] The present invention relates to a pretreatment method applied to different environmental media, more specifically for the combination of solvent extraction of composite organic extracts of water, sediment, soil, particulate matter and biological samples, column purification and step-by-step separation pre-processing method. Background technique [0002] In the past ten years, with the acceleration of industrialization and urbanization in our country, a large number of organic pollutants have entered into environmental media such as water, soil and the atmosphere. Most of these pollutants have the characteristics of low concentration, high toxicity and long-term retention in the environment. long. my country's environmental protection department has devoted a lot of energy to the monitoring of conventional organic pollutants (such as nitrobenzene and pesticides, etc.), and the routine detection of these compounds generally requires the support of larg...

Claims

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Application Information

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IPC IPC(8): G01N30/08
Inventor 于红霞史薇曹福苏冠勇韦斯
Owner NANJING UNIV
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