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A method for extracting and purifying phthalate plasticizers in vegetable oil

A technology of phthalic acid and vegetable oil, which is applied in the direction of instruments, measuring devices, scientific instruments, etc., can solve the problems of long detection time and cumbersome operation, and achieve the same detection limit, good reproducibility, and good application prospects Effect

Active Publication Date: 2021-04-16
浙江省林产品质量检测站
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the shortcomings of long detection time and cumbersome operation in the prior art, the present invention provides a method for extracting and purifying phthalic acid lipid plasticizers in vegetable oil

Method used

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  • A method for extracting and purifying phthalate plasticizers in vegetable oil
  • A method for extracting and purifying phthalate plasticizers in vegetable oil
  • A method for extracting and purifying phthalate plasticizers in vegetable oil

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Embodiment 1

[0026] A method for extracting and purifying PAEs plasticizers in vegetable oil, comprising the following steps:

[0027] (1) mix the camellia oleifera seed oil sample evenly, accurately weigh 1.00g vegetable oil sample and add in 10ml colorimetric tube 1;

[0028] (2) In the colorimetric tube 1 containing the vegetable oil sample, dichloromethane was added to set the volume to 10ml and mixed uniformly to obtain the extract 11;

[0029] (3) Draw 5ml of extraction solution 11 and pass through MycoSep 226AflaZon+column 2 to purify, after purification, above the purification column 21 of MycoSep226AflaZon+column 2, dichloromethane extract solution 22 is obtained;

[0030] (4) Take 0.5ml of dichloromethane extract solution 22 and put it into the sampling bottle, and use a mass spectrometer to measure and analyze the components and contents of phthalate plasticizers.

[0031] Chromatographic conditions of GC-MS:

[0032] Injection port: 250°C;

[0033] Injection volume: 1μl, spl...

Embodiment 2

[0045] A method for extracting and purifying phthalate plasticizers in vegetable oil, comprising the following steps:

[0046] (1) Mix the rapeseed oil sample evenly, accurately weigh 1.00g of the vegetable oil sample and add it to the 10ml colorimetric tube 1;

[0047] (2) In the colorimetric tube 1 containing the vegetable oil sample, dichloromethane was added to set the volume to 10ml and mixed uniformly to obtain the extract 11;

[0048](3) Draw 5ml of extraction solution 11 and pass through MycoSep 226AflaZon+column 2 for purification, after purification, above the purification column 21 of MycoSep226AflaZon+column 1, dichloromethane extraction solution 22 is obtained;

[0049] (4) Take 0.5ml of dichloromethane extract solution 22 and put it into the sampling bottle, and use a mass spectrometer to measure and analyze the components and contents of phthalate plasticizers.

[0050] Chromatographic conditions of GC-MS:

[0051] Injection port: 250°C;

[0052] Injection vo...

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Abstract

The invention relates to the field of plasticizer determination, and discloses a method for extracting and purifying phthalate plasticizers in vegetable oil. The steps include sampling vegetable oil, dissolving in dichloromethane, and extracting, and passing the extract (11) through MycoSep 226 After the AflaZon+ small column (2) is purified, put it into a sampling bottle and detect it with a gas chromatography-mass spectrometer. The pretreatment of the present invention is completed within 2 minutes, which greatly shortens the time used for conventional pretreatment; the cleanliness of the target extract is improved, the grease is fully removed to protect the detection equipment, the sensitivity of the equipment is consistent, and the detection limit remains unchanged. The recoveries of various concentrations of the target substance were all above 90%, and the relative standard deviation was within 5%. The solvent integrates dissolution and extraction, reduces the amount of organic reagents, and does not need to use concentration equipment, reduces the detection steps and manpower of conventional methods for such substances in vegetable oils, and improves detection efficiency; the method is used in vegetable oils and other The rapid detection of o-phthalic plasticizers in oil has a good application prospect.

Description

technical field [0001] The invention relates to the field of pretreatment of plasticizers, in particular to a method for extracting and purifying phthalate plasticizers in vegetable oil. Background technique [0002] Vegetable oil is an indispensable and important food material in people's daily life. It usually comes into contact with various plastic products during production, processing, storage and transportation, such as plastic pipes, plastic oil storage tanks, plastic packaging bottles, etc., mixed in these pipes PAEs in storage and transportation facilities will inevitably be incorporated into vegetable oil, causing oil pollution and ultimately endangering human health. [0003] Phthalate esters (Phthalate esters abbreviated as PAEs), also known as plasticizers, plasticizers, and titanates, are easily soluble in petroleum ether, methylene chloride, vegetable oil, etc. Appropriate application in plastic products can reduce their hardness , modulus, softening and embr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 杨柳朱杰丽王朝仁黄忆婷柴振林吴勋娅杨黎耀方燕吴翠荣周侃侃蒋步云尚素微
Owner 浙江省林产品质量检测站