Method for preparing bisphenol A molecular engram polymer

A molecular imprinting and polymer technology, applied in the field of new materials, can solve the problems of restricting the development of solid-phase extraction technology, complex cosmetic sample matrix, low content of target substances, etc., to achieve excellent recovery effect, high recovery rate and high sensitivity. Effect

Inactive Publication Date: 2008-05-14
HUBEI INSPECTION & QUARANTINE TECH CENT
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  • Abstract
  • Description
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Problems solved by technology

However, the matrix of cosmetic samples is complex, and the content of target substances is often relatively low. Therefore, how to effectively concentrate and enrich traces of bisphenol A drugs in cosmetic samples is a research hotspot in the field of cosmetic safety analysis.
At present, the most common treatment method is solid-phase extraction technology, but solid-phase extraction fillers include reversed-phase, normal-phase, ion-exchange and other types, including Cl8, C8, C2, -NH 2 , -Diol, -CN, Silica, Flofisil, alumina, polymer matrix, anion / cation exchange and DNPH and other adsorbents, but the interaction between the traditional solid phase extraction adsorbent and the target is non-specific, It is usually necessary to carefully select the extraction and elution conditions, so the separation and analysis of different matrices require the selection of different column packing materials, which limits the further development of solid phase extraction technology

Method used

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  • Method for preparing bisphenol A molecular engram polymer

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Comparison scheme
Effect test

Embodiment 1

[0016] Dissolve 9 mmol of template molecule bisphenol A and 6 mmol of functional monomer methacrylic acid into 12 mmol of crosslinker N,N′-methylenebisacrylamide, 40 mg of initiator azobisisobutyronitrile and 100 mL of Prepare a mixed solution from pure acetonitrile solution; ultrasonically degas the mixed solution for 6 minutes, pass nitrogen gas for 10 minutes to remove oxygen molecules, then seal the mixed solution, and polymerize by heating and stirring to form a white powder polymer at a polymerization temperature of 65°C , The reaction time is 20h. After the polymerization is completed, use a mixed solution of 100 mL of methanol and acetic acid with a volume ratio of 9:1 to extract the synthesized polymer by Soxhlet extraction to remove template molecules, and then use pure methanol to extract and remove acetic acid molecules. . After the extraction, the polymer was dried in a vacuum drying oven to a constant weight, and finally the bisphenol A molecularly imprinted pol...

Embodiment 2

[0018] Dissolve 10 mmol of template molecule bisphenol A and 6 mmol of functional monomer methacrylic acid into 12 mmol of crosslinker N,N′-methylenebisacrylamide, 40 mg of initiator azobisisobutyronitrile and 100 mL of Prepare a mixed solution from pure acetonitrile solution; ultrasonically degas the mixed solution for 6 minutes, pass nitrogen gas for 10 minutes to remove oxygen molecules, then seal the mixed solution, and polymerize by heating and stirring to form a white powdery polymer. The polymerization temperature is 65 °C, the reaction time is 20h. After the polymerization is completed, use a mixed solution of 100 mL of methanol and acetic acid with a volume ratio of 9:1 to extract the synthesized polymer by Soxhlet extraction to remove template molecules, and then use pure methanol to extract and remove acetic acid. molecular. After the extraction, the polymer was dried in a vacuum drying oven to a constant weight, and finally the bisphenol A molecularly imprinted po...

Embodiment 3

[0020] Dissolve 10mmol of template molecule bisphenol A and 6mmol of functional monomer acrylamide into a solution containing 12mmol of crosslinker N,N′-methylenebisacrylamide, 40mg of initiator azobisisobutyronitrile and 100mL of pure Prepare a mixed solution in an acetonitrile solution; ultrasonically degas the mixed solution for 6 minutes, pass nitrogen gas for 10 minutes to remove oxygen molecules, then seal the mixed solution, and polymerize by heating and stirring to form a white powdery polymer at a polymerization temperature of 65°C , The reaction time is 20h. After the polymerization is completed, use a mixed solution of 100 mL of methanol and acetic acid with a volume ratio of 9:1 to extract the synthesized polymer by Soxhlet extraction to remove template molecules, and then extract with pure methanol to remove Acetic acid molecule. After the extraction, the polymer was dried in a vacuum drying oven to a constant weight, and finally the bisphenol A molecularly impri...

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Abstract

The invention discloses a method for preparing bisphenol A molecular imprinting polymer, comprising the following procedures: dissolving template molecule bisphenol A and functional monomer according to the mol ratio of 1.5:1 to 2:1 into acetonitrile solution which is no less than 10ml with 10 to 15 crosslinking agent and initiator of catalytic amount to prepare mixed liquor; the mixture liquor is churned up at 55 to 70 DEG C to polymerize for 12 to 24 hours and then white powdery polymer is generated; synthesizing fine white powdery polymer using mixed solution of methanol and acetic acid as extracting solution, removing the template molecules and then extracting acetic acid molecules using pure methanol; after extracting, the polymer is arranged in vacuum drying chamber to dry until reaching balancing weight and then bisphenol A molecular imprinting polymer is obtained. The invention has advantages that the prepared bisphenol A molecular imprinting polymer has special adsorption for bisphenol A molecular in cosmetic samples which can rapidly, delicately and accurately concentrate and purify the cosmetic samples in an efficient way; the rate of recovery is high, the reproducibility is good and the sensitivity is high.

Description

technical field [0001] The invention relates to a preparation method of a bisphenol A molecularly imprinted polymer, which belongs to the field of new materials. Background technique [0002] The accumulation of bisphenol A, a hormone drug contained in cosmetics, in the human body can produce symptoms such as endocrine disorders, physical and psychological developmental disorders, teratogenicity, and reproductive system tumors. However, the matrix of cosmetic samples is complex and the content of the target substance is often relatively low. Therefore, how to effectively concentrate and enrich trace amounts of bisphenol A drugs in cosmetic samples is a research hotspot in the field of cosmetic safety analysis. At present, the most common treatment method is solid-phase extraction technology, but solid-phase extraction fillers include reversed-phase, normal-phase, ion-exchange and other types, including Cl8, C8, C2, -NH 2 , -Diol, -CN, Silica, Flofisil, alumina, polymer matr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/26C08F2/44C08F20/00C08F4/04C08F4/30C08K5/13
Inventor 林雁飞胡小钟王鹏
Owner HUBEI INSPECTION & QUARANTINE TECH CENT
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