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Preparation of p-hydroxybenzaldehyde enrichment reagent and products and applications

A p-hydroxybenzaldehyde and enrichment technology, applied in the polymer field, can solve the problems of narrow application range, few mobile phase types, complicated separation of large-scale precision instruments, etc., and achieves the effects of broad application prospects, simple operation and short time.

Inactive Publication Date: 2018-10-26
GUANGDONG GOLDEN LEAF TECH DEV +1
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  • Description
  • Claims
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Problems solved by technology

However, the above-mentioned methods all require the use of large-scale precision instruments and complicated separation in the early stage, and the purchase, use and maintenance costs of these instruments are generally high, so that the cost of the corresponding detection methods remains high
In addition, gas phase detection is affected by the stability and volatility of the sample, resulting in a narrow range of applications and fewer choices of corresponding mobile phases; while the detection time of liquid chromatography is relatively long

Method used

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  • Preparation of p-hydroxybenzaldehyde enrichment reagent and products and applications
  • Preparation of p-hydroxybenzaldehyde enrichment reagent and products and applications
  • Preparation of p-hydroxybenzaldehyde enrichment reagent and products and applications

Examples

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preparation example Construction

[0031] According to the first aspect of the present invention, in a preferred embodiment, the preparation method of p-Hydroxybenzaldehyde enrichment reagent comprises the following steps:

[0032] S1: Accurately weigh acrylic acid (0.2-0.3mmol), N-isopropylacrylamide, N,N-dimethylbisacrylamide, ultrasonically dissolve in 80mL water; then add N-tert-butylacrylamide in anhydrous Ethanol (1mL) solution, ultrasonic degassing for 10min;

[0033] S2: After adjusting the pH=6.0, adding p-hydroxybenzaldehyde as a template molecule;

[0034] Among them, the template molecules are added in the following molar ratios:

[0035] MIP-1: (acrylic acid: template molecule = 1:2)

[0036] MIP-2: (acrylic acid: template molecule = 1:4)

[0037] MIP-3: (acrylic acid: template molecule = 1:8)

[0038] MIP-4: (acrylic acid: template molecule = 1:16)

[0039] S3: Slowly add the aqueous solution of the initiator (ammonium persulfate, sodium bisulfite and sodium lauryl sulfate) dropwise, and poly...

Embodiment 1

[0048] Accurately weigh acrylic acid (0.2mmol), N-isopropylacrylamide (0.4mmol), N,N-dimethylbisacrylamide (2mmol) dissolved in 80mL distilled water, N-tert-butylacrylamide (0.2mmol) Dissolve in 1 mL of absolute ethanol, sonicate for 10 min; then, adjust pH=6.0 with NaOH, add 1.6 mmol template molecule (p-hydroxybenzaldehyde) (dissolved in distilled water), shake at 70 rpm at constant temperature (35°C) for 4 hours; then, slowly The aqueous solution of the initiator (ammonium persulfate (60.0mg), sodium bisulfite (20.0mg), sodium lauryl sulfate (40.0mg) dissolved in 20mL of distilled water) was added dropwise, and the polymerization reaction was carried out at 35°C for 24h;

[0049] After the reaction is complete, use ethanol-chloroform as the extractant, and use a Soxhlet extractor to reflux overnight to elute the template molecule (p-hydroxybenzaldehyde) to obtain a crude molecularly imprinted polymer;

[0050] The molecularly imprinted polymer crude product is dialyzed with...

Embodiment 2

[0054] ①Preparation of enrichment reagent solution (1mg / mL)

[0055] Accurately weigh 5.0 mg p-hydroxybenzaldehyde enrichment reagent MIP-3 and ultrasonically dissolve it in 5.0 mL of distilled water to prepare a 1 mg / mL enrichment reagent solution;

[0056] ②Determination of p-hydroxybenzaldehyde concentration-UV absorbance standard curve (0.1, 0.2, 0.5, 1.0, 2.0, 4.0, 5.0, 10.0μg / mL)

[0057] Purchase or prepare a standard solution of 100 μg / mL p-hydroxybenzaldehyde by yourself: Accurately weigh 2.0 mg of p-hydroxybenzaldehyde and dissolve it in 20.0 mL of absolute ethanol.

[0058] Preparation of 10μg / ml p-hydroxybenzaldehyde solution: 1ml 100μg / ml p-hydroxybenzaldehyde solution + 9ml absolute ethanol; preparation of 5μg / ml p-hydroxybenzaldehyde solution: 5ml 10μg / ml p-hydroxybenzaldehyde solution + 5ml anhydrous Ethanol; preparation of 4μg / ml p-hydroxybenzaldehyde solution: 2ml 10μg / ml p-hydroxybenzaldehyde solution + 3ml absolute ethanol; preparation of 2μg / ml p-hydroxyb...

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Abstract

The invention provides a preparation method of a p-hydroxybenzaldehyde enrichment reagent, the method includes the steps: acrylic acid, N-isopropyl acrylamide, N, N-dimethyl bis acrylamide is weighed,ultrasonically dissolved in water; N-tert-butyl acrylamide in anhydrous ethanol solution is added, ultrasonic degassing; after pH=5.8-6.2 is adjusted, p-hydroxybenzaldehyde is added as a template molecule; adding an aqueous solution of the initiator is added, polymerization; after the reaction is completed, the template molecule is eluted to prepare a crude molecularly imprinted polymer; the crude molecularly imprinted polymer is dialyzed, and then the dialyzate is lyophilized, the molecularly imprinted polymer solid powder is obtained, which is an enrichment of p-hydroxybenzaldehyde. The preparation method is simple in operation and low in cost, and is suitable for large-scale industrial production; and the p-hydroxybenzaldehyde enrichment reagent has a short adsorption time, and is suitable for tobacco quality control detection, and thus has broad application prospects.

Description

technical field [0001] The invention belongs to the technical field of macromolecules, and in particular relates to a preparation method of a p-hydroxybenzaldehyde enrichment reagent, a p-hydroxybenzaldehyde enrichment reagent prepared by the preparation method, and a preparation of the p-hydroxybenzaldehyde enrichment reagent application. Background technique [0002] Tobacco smoke contains more than 2,000 toxic substances, of which at least 69 are known carcinogens, including aldehydes, fused-ring aromatic hydrocarbons, N-nitrosoamines, aromatic amines and 1,3- Butadiene, etc., these carcinogens will cause gene mutations after being inhaled into the human body, and then lead to the occurrence of malignant tumors. Harmful gases such as nitric oxide, hydrogen sulfide and ammonia in tobacco smoke can cause serious harm to the respiratory system. Tobacco smoke also contains a variety of substances that can cause cardiovascular and cerebrovascular diseases, such as carbon mon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/38C08F220/54C08F220/06
CPCC08F222/385C08F220/54C08F220/06
Inventor 陈泽鹏傅源锋李正勇赵闯王磊管传莉陈桢禄文志强
Owner GUANGDONG GOLDEN LEAF TECH DEV
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