A kind of detection method of nitro polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in soil

A polycyclic aromatic hydrocarbons and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high professional requirements for operators, high requirements for instrumentation, time-consuming and labor-intensive problems, and achieve simple pre-treatment process, Less time-consuming, high-sensitivity effects

Active Publication Date: 2022-04-01
INST OF AGRO FOOD SCI & TECH CHINESE ACADEMY OF AGRI SCI
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Problems solved by technology

The application of physical and chemical analysis techniques such as chromatography and mass spectrometry to analyze trace amounts of nitro-PAH residues in environmental samples not only requires a high degree of instrumentation, but also requires pretreatment such as Soxhlet extraction, which is time-consuming and laborious. At the same time, professional requirements for operators Higher, the pretreatment process needs to use a large amount of organic solvents, which has caused new environmental pollution

Method used

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  • A kind of detection method of nitro polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in soil
  • A kind of detection method of nitro polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in soil
  • A kind of detection method of nitro polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in soil

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Embodiment 1

[0037] (1) Preparation of soil samples: 1 kg of soil samples were collected, ground after natural air drying, mixed evenly after passing through a 2mm sieve, and stored in a ventilated and dry place.

[0038] (2) Extraction: Weigh 10g of the soil sample in step (1), add 10ml of acetonitrile-saturated n-hexane to extract, vortex for 1min, add 4g of sodium chloride, vortex for 1min, ultrasonic for 15min, at a speed of 6000 rpm Centrifuge for 10 minutes, and take 2ml supernatant for later use.

[0039] (3) Purification: if figure 1 As shown, the 2ml supernatant taken out in step (2) was purified from the m-PFC column (filler was 2mg (MWCNTs)+30mgPSA+30mgC18+80mg MgSO 4 ) top, slowly push the plunger rod, that is, the purification is completed.

[0040] (4) Derivation: Dry the purified solution with nitrogen, then add 10 mg of iron powder and 0.2 mL of acetic acid methanol solution (the volume ratio of acetic acid and methanol is 3:17), shake for 20 minutes and then centrifuge a...

Embodiment 2

[0083] The difference between embodiment 2 and embodiment 1 is that the packing of the m-PFC purification column used for step (3) purification is different: the packing of embodiment 2 is 3mg (MWCNTs)+30mgPSA+30mgC18+80mg MgSO 4 .

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Abstract

The invention relates to a detection method of nitro polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in soil, comprising the following steps: (1) extraction: add n-hexane vortex to soil samples, centrifuge, and take supernatant; (2) purify and derivatization: pass the supernatant of step (1) through the m-PFC purification column and then dry it with nitrogen gas, and then react with the fluorescent derivatization reagent to generate a target substance with a fluorescent effect; (3) HPLC-FLD determination: use high-efficiency liquid The nitro polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in the target substance described in the step (2) are separated and detected by a phase chromatography-fluorescence detector coupling method. The present invention uses QuEChERS in combination with high performance liquid chromatography-fluorescence detector to propose a simple, fast and accurate detection technology for nitro polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in soil, which has strong specificity and high sensitivity, and can solve large The technology of polycyclic aromatic hydrocarbons and their nitro derivatives in batch samples has important practical significance.

Description

technical field [0001] The invention relates to the technical field of pollutant detection in soil, in particular to a detection method for nitro polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in soil. Background technique [0002] Nitro-PAHs are derivatives of PAHs, usually accompanied by parent PAHs, and their teratogenic and carcinogenic effects are stronger than those of the parent. For example, the typical nitro polycyclic aromatic hydrocarbon 1-nitropyrene is listed as a 2A carcinogen by the International Cancer Research Center (IARC), and its toxicity is 10-10 times that of the parent pyrene. 4 times. [0003] At present, the detection and analysis of polycyclic aromatic hydrocarbons in soil is mainly carried out by gas chromatography (GC), high performance liquid chromatography (HPLC) and tandem mass spectrometry, but there are few reports on the detection methods of nitro polycyclic aromatic hydrocarbons, mainly because The content of nitro ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06G01N30/34G01N30/74G01N30/14
CPCG01N30/88G01N30/06G01N30/34G01N30/74G01N30/14G01N2030/8854G01N2030/067
Inventor 邓凯琳黄亚涛李硕赵玉乐高彦琛张敏会范蓓王凤忠
Owner INST OF AGRO FOOD SCI & TECH CHINESE ACADEMY OF AGRI SCI
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