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Determination methods of 6 kinds of phthalates in soil

A technology for phthalate esters and determination methods, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of column loss, low sensitivity, complicated pretreatment, etc., and achieve the reduction of pollution introduction, simplified operation, and recovery high rate effect

Active Publication Date: 2020-02-11
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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Problems solved by technology

[0007] The pretreatment method of QuEChERs has also been reported, but it is mainly used in combination with liquid chromatography, and there are few reports on the combination with gas chromatography. This is because QuEChERs often use acetonitrile as a simple solvent to extract samples, and direct injection of acetonitrile is not suitable for gas chromatography. The main phenomenon of non-polar columns commonly used for dicarboxylates is severe column loss and more interference from fragment ions. Therefore, if QuEChERs is used, the last step is mostly solvent conversion (conversion of polar solvents such as acetonitrile into non-hexane, etc. polar solvents)
However, the sensitivity of liquid chromatography with PDA detector is low; moreover, the overall polarity of ortho-phenyl esters is relatively weak. Chemical ionization (APCI) source, and many standard methods (ISO 13913-2014) issued by ISO and US EPA all use GC-MS with non-polar column to measure samples, but the pretreatment is more complicated

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  • Determination methods of 6 kinds of phthalates in soil
  • Determination methods of 6 kinds of phthalates in soil
  • Determination methods of 6 kinds of phthalates in soil

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Embodiment

[0052] Example: Determination of 6 kinds of phthalates in soil.

[0053] (1) The collected soil samples were naturally air-dried, ground, and passed through a 0.25 mm sieve.

[0054] (2) Accurately weigh 1.5-2.5g of sample, accurate to 0.0001g, into a 30mL glass centrifuge tube, add 2mL of water, vortex for 1min to infiltrate the water and sample, add 3-5mL of acetonitrile, 100µL internal standard, vortex 1.5min, add n-hexane and ethyl acetate mixed solution, then add 2g MgSO 4 , then vortexed for 1min, centrifuged at 4000r / min for 3min, sucked 1.5-2mL of the supernatant into a 10mL glass centrifuge tube with a glass pipette, and added dispersive solid phase extraction reagents (50mg PSA, 50mg C18EC, 150mg MgSO 4 ), vortex for 1min, centrifuge at 4000r / min for 2min, and take the supernatant for analysis.

[0055] (3) Determination of samples by GC-MS. The analysis conditions are:

[0056] Gas Chromatography Conditions

[0057] Analytical column: capillary column: stationa...

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Abstract

The invention belongs to the field of physical and chemical analysis of environment samples (soils), and concretely relates to a method for determining six phthalates in soil. The method comprises thefollowing steps: preprocessing a sample by a QuEChREs technology, extracting the sample by using an acetonitrile, n-hexane and ethyl acetate mixed solvent, purifying the sample by using a matrix dispersion solid-phase extraction kit, and determining the phthalates in the soil sample by using gas chromatography-mass spectrometry. The method has the advantages of simplicity and fastness in pretreatment, high determination efficiency, suitableness for GC-MS determination, and accurate determination result.

Description

technical field [0001] The invention belongs to the field of physical and chemical analysis of environmental samples (soil), in particular to the determination of six phthalate compounds in soil. Background technique [0002] Phthalates, also known as phthalates, abbreviated as PAEs, are currently widely used in various industries closely related to human production and life. Since PAEs do not form stable chemical bonds with the polymer matrix in plastics, coatings, etc., they are easy to migrate from them after use, causing pollution and may be passed to the human body through the food chain. In the past, it was always believed that the toxicity of plasticizers was very low, but recent studies have shown that o-phenyl esters can cause functional changes in the central nervous system and peripheral nervous system, showing strong endocrine disrupting properties, and are an environmental hormone with teratogenic properties. , carcinogenic and mutagenic hazards. [0003] Exte...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/062
Inventor 王颖边照阳张仕祥杨飞刘珊珊邓惠敏李中皓范子彦唐纲岭
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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