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Method for measuring hydroxy polybrominated diphenyl ether in plant samples

A hydroxy polybrominated diphenyl ether and sample technology, applied in the detection field, can solve the problems of inaccurate quantitative results, affecting OH-PBDEs, and low selectivity, and achieve the effects of reducing the impact of detection results, improving accuracy and high sensitivity

Active Publication Date: 2019-04-05
NORTHWEST UNIV(CN)
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Problems solved by technology

[0004] At present, the detection method of OH-PBDEs in biological samples mainly adopts gas chromatography-mass spectrometry to analyze the methoxypolybrominated diphenyl ethers (MeO-PBDEs) of its derivatized products. The derivatization step is very time-consuming, the pretreatment of the sample is very cumbersome, and the derivatization reagents are usually dangerous, and incomplete derivatization will also lead to inaccurate quantitative results. In recent years, due to the liquid chromatography-mass spectrometry (LC-MS ) does not require derivatization treatment, and has the advantages of high sensitivity, superior separation ability, and simplicity and speed. It is widely used in the field of environmental analysis and has gradually become an important analytical method.
However, the existing LC-MS analysis methods for OH-PBDEs are mainly for animal tissue and blood samples, and the extraction and determination of plant samples have not been reported. In addition, for the detection of OH-PBDEs in plant samples, due to the There are often a large amount of impurities such as chlorophyll and lipids in the plant, which will affect the results of OH-PBDEs in mass spectrometry detection. Therefore, it is the key to determine the content of OH-PBDEs in plants to be able to effectively remove impurities such as chlorophyll and lipids in the pre-treatment part. The premise is that most of the existing methods for removing chlorophyll use activated carbon adsorption, but the selectivity of activated carbon adsorption is not high, and it is easy to adsorb other useful substances, resulting in inaccurate analysis results

Method used

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  • Method for measuring hydroxy polybrominated diphenyl ether in plant samples
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  • Method for measuring hydroxy polybrominated diphenyl ether in plant samples

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preparation example Construction

[0032] Preparation of porous magnetic ferric oxide: under the protection of nitrogen, take 20g of 1.0mmol / g FeSO 4 ·7H 2 O and 40 g FeSO at 2.0 mmol / g 4 ·6H 2 O was added to 1000mL ethylene glycol, stirred until the solid was dissolved, then added 100g of dodecylamine (surfactant), stirred at 300rpm and 25°C for 10min, added 20g of ammonium acetate, continued to stir for 30min, and then continued stirring to add 15g of sodium citrate, stirred at 500rpm until the suspension becomes a uniform solution, put it in a stainless steel reactor, place the reactor in an oven and heat it to 200°C, keep it warm for 10h, then cool down to room temperature, then Centrifuge at a speed of 10000r / min for 5min, wash with ethanol and deionized water, and dry in vacuum at a vacuum degree of -0.06MPa and a temperature of 60°C to obtain porous magnetic ferric oxide;

[0033]Coating: Take 60g of porous magnetic ferric ferric oxide and place it in 1000mL of methanol solution, then add 180g of need...

Embodiment 1

[0039] Extraction: cut the freeze-dried plant sample into pieces, accurately weigh 3.0g (dry weight), add 2mL, 37wt% HCl solution and 10mL isopropanol to mix, then add 3mL n-hexane-MTBE mixed solution A ( The volume ratio of n-hexane to MTBE in n-hexane-MTBE mixed solution A is 1:1), ultrasonically oscillated for 24 hours, centrifuged at a speed of 10000rpm, removed once to extract the organic phase, precipitated and repeated all the above operations, combined twice and once extracted the organic phase phase to obtain the crude extract;

[0040] Secondary extraction: After drying the organic phase in the crude extract with nitrogen, dissolve it in 2 mL of n-hexane, add 1 mL of NaOH solution for extraction (the NaOH solution is obtained by dissolving 0.5 mol / L NaOH in 50% ethanol), and separate to obtain Extract the organic phase and the aqueous phase twice, add 2mL n-hexane to the aqueous phase to extract the aqueous phase again, then add 300μL, 2M HCl solution, and extract th...

Embodiment 2

[0045] Extraction: Cut the freeze-dried plant sample into pieces, accurately weigh 4.0g (dry weight), add 3mL, 37wt% HCl solution and 15mL isopropanol and mix well, then add 4.5mL n-hexane-MTBE mixed solution A (The volume ratio of n-hexane to MTBE in n-hexane-MTBE mixed solution A is 1:1), ultrasonically oscillated for 24 hours, centrifuged at a speed of 10000rpm, removed once to extract the organic phase, precipitated and repeated all the above operations, combined twice and once extracted The organic phase obtains a crude extract;

[0046] Secondary extraction: After the organic phase in the crude extract was blown dry with nitrogen, it was dissolved in 3mL of n-hexane, and 1.5mL of NaOH solution was added for extraction (the NaOH solution was obtained by dissolving 0.5mol / L NaOH in 50% ethanol), and separated To obtain the secondary extraction of the organic phase and the aqueous phase, add 3 mL of n-hexane to the aqueous phase to extract the aqueous phase again, then add ...

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Abstract

The invention relates to the field of detection technology, in particular to a method for measuring the hydroxy polybrominated diphenyl ether in a plant sample. The method comprises extraction, secondary extraction, chlorophyll removal, purification, and analysis. The analysis method uses a combined analysis method using ultra-high performance liquid chromatography-electrospray ion source-series triple quadrupole mass spectrometer combined analysis method. The chlorophyll removal uses a nano magnetic molecular material as a selective adsorbent. The method for measuring hydroxy polybrominated diphenyl ether in plant samples uses the method of ultra-high performance liquid chromatography-electrospray ion source-series triple quadrupole mass spectrometer combined analysis method, which is simple, rapid and sensitive. Therefore the separation of OH-PBDEs homologs and isomers can be well achieved, and their accurate qualitative and quantitative analysis can be achieved. And magnetic molecularly imprinted material is used as a selective adsorbent in the process, which has higher selectivity and better adsorption effect.

Description

technical field [0001] The invention relates to the technical field of detection, in particular to a method for determining hydroxy polybrominated diphenyl ethers in plant samples. Background technique [0002] Polybrominated diphenyl ethers (PBDEs), an important new type of brominated flame retardant, are widely used in the fields of plastics, electrical appliances, furniture, textiles and chemicals because of their high flame retardant efficiency, good thermal stability, and low impact on material properties. At the same time, PBDEs are a kind of global organic pollutants that widely exist in the environment. On the one hand, because PBDEs have the characteristics of low vapor pressure and strong lipophilicity at room temperature, they can be dissipated into the air and transported with the atmosphere for long distances. On the other hand, they are Because of its stable chemical properties, it may bioaccumulate and amplify along the food chain, and it is bioaccumulative. A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 王森
Owner NORTHWEST UNIV(CN)
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