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Preparation method of reusable solid-phase extraction material based on beta-cyclodextrin

A solid-phase extraction material, β-cyclodextrin technology, applied in the field of environmental chemistry and analysis and detection, can solve the problems of insufficient sensitivity of the instrument, low target content, inaccurate determination, etc.

Inactive Publication Date: 2020-10-20
INSPECTION & QUARANTINE TECH CENT OF FUJIAN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of a reusable solid phase extraction material based on β-cyclodextrin, which can not only efficiently and quickly separate and enrich the target, but also solve the problem of complex matrix and target in the actual detection work. The content is too low, the sensitivity of the instrument is not up to the problem of inaccurate determination, and this kind of solid phase extraction agent can be regenerated and reused, which can save testing costs and reduce experimental waste. It is suitable for quality control and circulation of enterprise production. Quality control in the field and regulatory control of related product safety

Method used

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  • Preparation method of reusable solid-phase extraction material based on beta-cyclodextrin
  • Preparation method of reusable solid-phase extraction material based on beta-cyclodextrin
  • Preparation method of reusable solid-phase extraction material based on beta-cyclodextrin

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preparation example Construction

[0028] A method for preparing a reusable solid phase extraction material based on β cyclodextrin, the specific steps are as follows:

[0029] (1) Add 0.10-0.50mol β-cyclodextrin, 0.10-0.50mol benzene-containing halide, 0.10-0.50mol carbonate in a flame-dried scintillation counting flask, and fill with nitrogen for 5 minutes;

[0030] (2) Add 5-10 mL of organic solvent A, 0.1-0.3 mol of initiator, and fill with nitrogen for 5 minutes;

[0031] (3) Turn off the nitrogen and react for 36-72h under the conditions of 70-90℃ and stirring speed of 300-500 r / min;

[0032] (4) Wash the polymer synthesized by the reaction with 1M acid until there is no bubbling, then wash with deionized water several times, then wash with organic solvent A twice, and organic solvent B twice;

[0033] (5) The polymer after washing is vacuum dried at 40°C for 24h, or liquid nitrogen at -196°C for 10min to prepare β-cyclodextrin polymer which can be used as solid phase extraction material.

[0034] Wherein, the benze...

Embodiment 1

[0042] (1) Add 0.10mol β-cyclodextrin, 0.10mol tetrachloroterephthalonitrile, and 0.10mol calcium carbonate to a flame-dried scintillation counting flask, and fill with nitrogen for 5 min;

[0043] (2) Add 5 mL of butyl acetate, 0.1 mol of benzophenone, and fill with nitrogen for 5 minutes;

[0044] (3) Turn off the nitrogen, and react for 36 hours at 70°C and a stirring speed of 400 r / min;

[0045] (4) Wash the polymer synthesized by the reaction with 1M acid until no bubbling, then wash it with deionized water several times, then wash it with butyl acetate twice, and wash it twice with diethyl ether;

[0046] (5) The polymer after washing is vacuum dried at 40°C for 24 hours to prepare β-cyclodextrin polymer which can be used as solid phase extraction material.

Embodiment 2

[0048] (1) Add 0.20mol β-cyclodextrin, 0.30mol decafluorobiphenyl, 0.15mol sodium carbonate to a flame-dried scintillation counting flask, and fill it with nitrogen for 5 minutes;

[0049] (2) Add 6 mL of propanol, 0.2 mol of azobisisobutyronitrile, and fill with nitrogen for 5 minutes;

[0050] (3) Turn off the nitrogen, and react for 72 hours at 80°C and a stirring speed of 300 r / min;

[0051] (4) Wash the polymer synthesized by the reaction with 1M acid until there is no bubbling, then wash it with deionized water several times, then wash it twice with propanol and twice with isobutanol;

[0052] (5) Dry the polymer after washing with liquid nitrogen at -196°C for 10 minutes to prepare β-cyclodextrin polymer that can be used as a solid phase extraction material.

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Abstract

The invention discloses a preparation method of a reusable solid-phase extraction material based on beta-cyclodextrin, which comprises the following steps: reacting beta-cyclodextrin, benzene-containing halide, carbonate and initiator in an organic solvent under nitrogen conditions, pickling, washing with water, washing with a solvent, and drying to obtain the beta-cyclodextrin polymer used as thesolid-phase extraction material. The method is simple in process and low in cost; the obtained solid-phase extraction material can be used for selective separation and enrichment of target objects inenvironmental samples, consumer goods and industrial products, serious interference of matrixes can be avoided, the problem of inaccurate measurement caused by too low content of the target objects and incapability of reaching sensitivity of instruments in current detection work is solved, and the material can also be repeatedly used.

Description

Technical field [0001] The invention belongs to the technical field of environmental chemistry and analysis and detection, and specifically relates to a method for preparing a reusable solid phase extraction material based on beta cyclodextrin. Background technique [0002] β-cyclodextrin has good emulsifying and dispersing properties, can reduce volatilization, reduce toxicity, improve solubility, and is also very excellent in terms of moisture-proof and moisturizing and prolonging the efficacy of preparations. β-cyclodextrin is extracted from natural polymer materials and has the characteristics of wide sources, low toxicity, low production cost, and biodegradability. Modification of it can obtain better characteristics and greatly improve the application effect. Therefore, β-cyclodextrin, as a clean and green carrier material, has the advantages of non-toxic, odorless and harmless to the human body, and has a wide range of applications in the fields of medicine, food, and wate...

Claims

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Application Information

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IPC IPC(8): C08B37/16C08J9/26B01J20/285C08L5/16
CPCB01J20/285C08B37/0012C08J9/26C08J2201/0444C08J2305/16
Inventor 戴金兰尹洪雷程立军丁立平梁震唐泓涂满娣俞凌云周磊
Owner INSPECTION & QUARANTINE TECH CENT OF FUJIAN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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