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Method for utilizing matrix solid-phase dispersion extraction to analyze plant organophosphorus ester

An organic phosphate ester and matrix solid-phase technology, which is applied in the direction of analyzing materials, material separation, measuring devices, etc., can solve problems such as analysis methods that are rarely reported, achieve good purification effect, low method detection limit and quantification limit, and improve selection Effects on Sex and Sensitivity

Active Publication Date: 2018-09-11
丹东龙泽化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there have been many reports on the analysis methods of organophosphates in samples such as air, water, soil, and sediment, but there are few reports on the analysis methods for plant samples.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The present invention is used to analyze organic phosphate in rapeseed.

[0028] 1. Break the rapeseed sample with a high-speed tissue grinder;

[0029] 2. Accurately weigh 0.5 g of the crushed rapeseed sample in step 1 and put it into a glass mortar, add 20 ng of substitution compound, 2 g of anhydrous sodium sulfate baked at 450 °C for 4 hours, 0.1 g of graphitized carbon black and 2 g of florisil after activation at 400 °C for 8 hours and deactivated with 3% deionized water by weight, milled for 10 min;

[0030] 3. Transfer the homogeneously ground mixture in step 2 to the empty SPE column that has been placed in the sieve plate, cover the sieve plate and compact it with a syringe plunger;

[0031] 4. Wash the mortar and pestle in step 2 three times with 15 mL of n-hexane and acetone mixed solution with a volume ratio of 1:1, and then transfer to the solid phase extraction column in step 3 to elute the target compound by gravity flow ;

[0032] 5. Collect the elua...

Embodiment 2

[0040] The present invention is used to analyze organic phosphates in potatoes.

[0041] 1. Break the rapeseed sample with a high-speed tissue grinder;

[0042] 2. Accurately weigh 0.5 g of the crushed rapeseed sample in step 1 and put it into a glass mortar, 2 g of anhydrous sodium sulfate baked at 450 °C for 4 hours, 0.1 g of graphitized carbon black and 2 g at 400 °C After activation for 8 hours at C and deactivated florisil with a weight ratio of 3% deionized water, grind for 20 min;

[0043] 3. Transfer the homogeneously ground mixture in step 2 to the empty SPE column that has been placed in the sieve plate, cover the sieve plate and compact it with a syringe plunger;

[0044] 4. Wash the mortar and pestle in step 2 three times with 20 mL of n-hexane and acetone mixed solution with a volume ratio of 1:1, and then transfer to the solid-phase extraction column in step 3 to elute the target compound by gravity flow ;

[0045] 5. Collect the eluate in step 4 and concentra...

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PUM

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Abstract

The invention discloses a method for utilizing matrix solid-phase dispersion extraction to analyze plant organophosphorus ester and relates to a plant organophosphorus ester analyzing method. The method comprises the steps: cutting up a plant sample, grinding the plant sample with an adsorbent, transferring a mixture into an empty solid-phase extracting column, eluting the solid-phased extractioncolumn, collecting and concentrating eluant, utilizing a solvent to dissolve the eluant, then utilizing a gas chromatography-serial triple quadrupole mass spectrum to perform qualitative and quantitative analysis on 13 kinds of organophosphorus ester. In the method disclosed by the invention, the sample is extracted and purified at the same time, an operation process is simple, an organic solventuse amount is small, a sample use amount is smaller, and consumed time is short; by means of the gas chromatography-serial triple quadrupole mass spectrum, selectivity and flexibility of target compound are improved; an adding standard recovery rate of the 13 kinds of organophosphorus ester is 65.1% to 109.1%, relative standard deviation is smaller than 15%, and good accuracy and precision are achieved; a detection limit of the method is 0.05ng / g to 0.33ng / g, a quantitation limit of the method is 0.16ng / g to 1.10ng / g, and the method can be applied to trace analysis.

Description

technical field [0001] The invention relates to a method for analyzing plant organophosphates, in particular to a method for analyzing plant organophosphates by matrix solid-phase dispersion extraction. Background technique [0002] In the production process of plastic products, in order to improve its quality and reduce its burning risk, it is often necessary to add flame retardants and plasticizers. Polybrominated diphenyl ethers (PBDEs) and organophosphate esters (OPEs) are the two most widely used plastic additives. The use of PBDEs has been banned due to their persistence, bioaccumulation and toxicity. OPEs are widely used as its substitutes. However, OPEs are not safe, and many studies have shown that organophosphates have potential biotoxic effects and can be enriched in organisms. For example, tris(2-chloroethyl) phosphate can cause brain and liver damage and cause cancer in rats, tris(2-chloroisopropyl) phosphate and tris(1,3-dichloroisopropyl) phosphate Can sig...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 罗庆王诗雨单岳孙丽娜王辉
Owner 丹东龙泽化工有限责任公司
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