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A method for fast separation of phthalates by supercritical chromatography

A phthalic acid and supercritical chromatography technology, which is applied in the field of rapid separation of phthalates by supercritical chromatography, can solve the problems of inconvenience, toxic and environmentally friendly solvents, etc., and achieves reduced use, shortened separation time, and rapid separation. The effect of detection

Inactive Publication Date: 2018-08-14
CHONGQING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0022] The present invention is aimed at the shortcomings of the current phthalate plasticizers, such as long separation time, toxic solvents, environmental protection, and no economy, etc., and proposes a new method for separating phthalate plasticizers in a short time by supercritical chromatography technology , this method has the advantages of rapidity, good reproducibility, simple operation, less solvent usage, green and environmental protection, etc.

Method used

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  • A method for fast separation of phthalates by supercritical chromatography
  • A method for fast separation of phthalates by supercritical chromatography

Examples

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Effect test

Embodiment 1

[0039] Since the plasticizer is contained in the plastic, the whole experiment process cannot touch the plastic-containing products. All glass instruments need to be soaked in acetone for 1 hour, and taken out of the oven after 2 hours for later use.

[0040] with CO 2 As mobile phase, acetonitrile as auxiliary agent; elution gradient was initially 100% CO 2 , change to 98% in one minute, change to 80% in 6 minutes, hold for 2 minutes, return to 98% in half a minute, and use half a minute to 100% CO 2 The temperature of the chromatographic column is 65°C; the flow rate is 1.5ml / min; the back pressure is 1800psi; the solution containing phthalates can be separated according to the above conditions, and more than a dozen target substances can be separated within a few minutes.

Embodiment 2

[0042] Since the plasticizer is contained in the plastic, the whole experiment process cannot touch the plastic-containing products. All glass instruments need to be soaked in acetone for 1 hour, and taken out of the oven after 2 hours for later use.

[0043] with CO 2 As mobile phase, isopropanol as auxiliary agent, according to the elution concentration of initial 96% CO 2 , maintain a constant volume ratio for 5 minutes, and reach 80% CO in 8 minutes 2 , back to 100% CO in 9 minutes 2The temperature of the chromatographic column is 65°C; the flow rate is 1.5ml / min; the back pressure is 1800psi, and the target substance can be separated in a few minutes. Compared with Example 1, the retention time is different.

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Abstract

The invention discloses a method for supercritical fluid chromatography-based fast separation of phthalate and belongs to the technical field of separation. The fast, saving and eco-friendly method provided through the invention solves the problem that the existing fluid chromatography or gas chromatography method for separating a phthalate plasticizer consumes long time and a large amount of materials. The method utilizes a supercritical fluid chromatography method to separate a desired substance, utilizes a CO<2+> adjuvant as a mobile phase, realizes separation of more than ten kinds of phthalate plasticizers in several minutes, is fast and eco-friendly, is poisonless and harmless for an experimenter and has good reappearance. Through combination of the method and UV, FID and MS detecting instruments, fast separation and detection of phthalate plasticizers are realized.

Description

1. Technical field [0001] The invention relates to a method for quickly separating phthalates by supercritical chromatography, belonging to the technical field of separation and analysis 2. Background technology [0002] Phthalate is an additive added to materials to make it elastic and soft. It can also be called phthalate plasticizer or plasticizer. It is widely used in national industries such as food and chemical industry. For example: food plastic packaging bags, cosmetic packaging, stationery and so on. At present, there are many types of plasticizers at home and abroad, including phthalates, aliphatic dibasic acid esters, phosphates, epoxy compounds, etc. Among them, phthalates are the most widely used. class of plasticizers (PAEs). After the "clouding agent" incident in Taiwan in May 2011 and the baijiu incident in 2012, the country has drawn strong attention to plasticizers. [0003] Phthalate plasticizers are an environmental hormone that acts very similarly to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 李泽全李雪敏卢姣但林阳刘楠胡玲
Owner CHONGQING UNIV
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