Method for analyzing phthalate in soil based on gas chromatography-mass spectrometry of microwave extraction
A phthalic acid and GC-MS technology, which is applied in the field of soil monitoring, can solve problems affecting the health of analysts, consume a large amount of organic solvents, and low automation, and achieve high automation, accurate analysis results, and time-saving costs. Effect
Pending Publication Date: 2020-11-13
NANJING BAIYUN CHEM ENVIRONMENTAL MONITORING
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[0003] At present, there is no domestic authoritative standard for the analysis method of phthalates in soil. The pretreatment method is generally Soxhlet extraction, which takes a long time, troublesome operation, low degree of automation, large amount of organic solvent, and solvent volatilization affects the health of analysts.
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[0018] A method for analyzing phthalates in soil by gas chromatography-mass spectrometry based on microwave extraction, the specific steps are as follows:
[0019] 1. Steps of microwave extraction pretreatment:
[0020] Take 5-10g of the collected soil sample and add anhydrous sodium sulfate to mix, dehydrate, grind and mix until it becomes granular; put the soil to be tested into a microwave extraction tank, add 100ml of n-hexane / acetone mixed solvent (1:1) , seal the extraction tank and put it into the microwave extractor, set the preheating time for 5 minutes, extract the temperature at 110°C, and extract for 10 minutes to perform extraction; after the extraction is completed and cooled, pass the extract through a sand core filled with anhydrous sodium sulfate Filter the funnel to remove water, concentrate to 1ml with a concentrator, purify and wash the concentrated solution through a magnesium silicate solid-phase extraction column, collect the eluate and concentrate it to...
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Abstract
The invention relates to a method for analyzing phthalate in soil by gas chromatography-mass spectrometry based on microwave extraction. The method comprises the following steps of step 1, adding anhydrous sodium sulfate into a collected soil sample, uniformly mixing, dehydrating, grinding and uniformly stirring to obtain granular soil; step 2, putting the to-be-detected soil treated in the step 1into a microwave extraction tank, adding an n-hexane / acetone mixed solvent, and adopting a microwave extractor to set extraction conditions for extraction; step 3, filtering and concentrating the extracting solution obtained in the step 2, purifying through a solid-phase extraction column, and concentrating for later detection; and step 4, putting the to-be-detected liquid treated in the step 3 into a gas chromatograph-mass spectrometer for analysis. The microwave extraction pretreatment method has the advantages of being high in automation degree, capable of saving time and cost, high in extraction efficiency and accurate in analysis result, and is an efficient pretreatment method, a gas chromatograph-mass spectrometer is adopted to analyze and test the sample, so analysis accuracy is high, and the method is quick and sensitive.
Description
technical field [0001] The invention relates to a method for testing and analyzing phthalates in the field of soil monitoring, in particular to a method for analyzing phthalates in soil by gas chromatography-mass chromatography based on microwave extraction. Background technique [0002] Phthalates, also known as phthalates, are widely used in packaging materials, cosmetics, toys, detergents and other products. Long-term exposure can interfere with human endocrine and directly harm the human reproductive system. [0003] At present, there is no domestic authoritative standard for the analysis method of phthalates in soil. The pretreatment method is generally Soxhlet extraction method, which takes a long time, troublesome operation, low degree of automation, large amount of organic solvent, and solvent volatilization affects the health of analysts. It is urgent to find a more efficient and convenient pretreatment method that can replace the traditional method. Contents of t...
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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 曹家平朱文静王海珍丁海霞
Owner NANJING BAIYUN CHEM ENVIRONMENTAL MONITORING