CN102443101A - Yohimbine detection material prepared by utilizing methacrylic acid and preparation method thereof - Google Patents
Yohimbine detection material prepared by utilizing methacrylic acid and preparation method thereof Download PDFInfo
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- CN102443101A CN102443101A CN201110331067XA CN201110331067A CN102443101A CN 102443101 A CN102443101 A CN 102443101A CN 201110331067X A CN201110331067X A CN 201110331067XA CN 201110331067 A CN201110331067 A CN 201110331067A CN 102443101 A CN102443101 A CN 102443101A
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- yohimbine
- template molecule
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- imprinted polymer
- linking agent
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Abstract
The invention relates to a yohimbine molecular imprinted polymer and a preparation method thereof. The preparation method comprises the following steps of: dissolving a functional monomer namely methacrylic acid and a template molecule namely yohimbine in dimethyl sulfoxide, mixing at room temperature for 6-24 hours, then adding ethylene glycol dimethacrylate serving as a cross-linking agent and an initiator, ultrasonically degassing, introducing nitrogen for removing oxygen, sealing, carrying out thermal-initiated polymerization and cleaning to remove the template molecule. According to the invention, the yohimbine molecular imprinted polymer is prepared by utilizing molecular recognition capability of a molecular imprinting technique, and a better recognition effect is obtained by optimizing the ratio of various raw materials.
Description
Technical field
The invention belongs to the foodstuff additive detection range, belong to especially and utilize molecular imprinting to detect Yohimbine.
Background technology
Yohimbine (Yohimbine) has the energy metabolism of the human body of acceleration, increases the effect that energy is supplied with.The product that contains Yohimbine has been issued ban by Czech Republic's agricultural and food quarantine office at present, forbids being used for athletic food and foodstuff additive.Therefore need detect Yohimbine in food or the foodstuff additive.
Molecular imprinting is the technology that a kind of preparation has the molecule distinguishability polymkeric substance.The preparation molecularly imprinted polymer generally needs three processes: (1) microsphere (being identified material) and function monomer interact, and form mixture; (2) through linking agent, microsphere with carry out polyreaction around the function monomer mixture, formation has macropore, netted polymkeric substance; (3) choosing appropriate means removes microsphere and just can obtain molecularly imprinted polymer.Exist with microsphere in the molecularly imprinted polymer for preparing like this and mate fully, and contain the three-dimensional hole with microsphere complementary function group at space structure.
Molecularly imprinted polymer is widely used in fields such as biology, medical science, chemistry with its good performance.With the theophylline content among the polymer determination patients serum of theophylline trace, the mensuration result of the same enzyme immunoassay of gained result (EMIT) is consistent.Molecular imprinting transmitter even can detect the microsphere of 1～50 μ mol, visible selectivity and susceptibility with height.Molecular imprinting can carry out trace to any material in theory, and the Yohimbine that therefore adopts molecular imprinting to detect in the feed has very big potential quality.
Summary of the invention
The objective of the invention is to prepare a kind of molecularly imprinted polymer that is used to detect Yohimbine, can reach good Yohimbine and detect effect.
The preparation method of Yohimbine molecularly imprinted polymer provided by the invention may further comprise the steps:
Function monomer methylacrylic acid and template molecule Yohimbine are dissolved in the methyl-sulphoxide, mixed at room temperature 6-24 hour, add linking agent TGM 1 and initiator then; Ultrasonic degas; Logical nitrogen deoxygenation, sealing back thermal-initiated polymerization is cleaned and is removed template molecule.
Wherein the mol ratio of template molecule and function monomer is: 1: 1-10, preferred 1: 1-8, more preferably 1: 4-8, most preferably 1: 6.
Wherein the mol ratio of template molecule and linking agent is: 1: 5-30, preferred 1: 10-25, most preferably 1: 20.
Wherein the mol ratio of function monomer, template molecule and linking agent is: 6: 1: 20.
At least 5 minutes ultrasonic degas time wherein.
At least 5 minutes oxygen deoxygenation time wherein.
Adopt the mixing solutions cleaning of methyl alcohol and acetate to remove template molecule.
Wherein the volume ratio of methyl alcohol and acetate is 1: 9.
The present invention provides a kind of Yohimbine molecularly imprinted polymer, and it adopts method for preparing to obtain.
The effect that the present invention reaches:
Utilize the molecule distinguishability of molecular imprinting, prepared the Yohimbine molecularly imprinted polymer, obtained recognition effect preferably through optimizing various material rates.
Embodiment
Embodiment 1
Accurately taking by weighing function monomer methylacrylic acid 4mmol and template molecule Yohimbine 1mmol is dissolved in the 25ml methyl-sulphoxide (DMSO); Mix 12h under the room temperature, function monomer and template molecule are fully acted on, add linking agent TGM 1 (EGDMA) 25mmol and 50mg initiator Diisopropyl azodicarboxylate (AIBN) then; Ultrasonic degas 10 minutes; Fed nitrogen 10 minutes, the vacuum lower seal, polymerization 48h obtains molecularly imprinted polymer in 60 ℃ of airbaths.
Molecularly imprinted polymer is pulverized the back grinds screening, get the particle (granularity 30.8～38.5 μ m) between 400 orders and 500 orders, with acetone repeatedly suspension settlement remove fine powder.The 1.5g polymer dispersed in the ethanol homogenate, under the pressure of 28MPa, is made displacing liquid with ethanol, adopt wet method to pack into and be of a size of: in the chromatographic column of 250mm * Φ 4mm.
Populated chromatographic column is used methyl alcohol: acetate=1: 9 (V: eluant solution V), analyze with HPLC, UV detector wavelength 268nm walks flatly to baseline, and it is complete to think that microsphere advances this wash-out.
In the experiment, measure the dead time with acetonitrile, retention factors k=(t-t0)/t0, t are the RT of analyte, and t0 is the dead time.Selectivity factor α=k1/k2, k1 are the retention factors of Yohimbine, and k2 is the retention factors of Yohimbine analogue.Chromatographic condition: acetonitrile is a moving phase, 27 ℃ of column temperatures, and flow velocity 0.3ml/min tests for the Yohimbine analogue with the serpentine.
Embodiment 2-9
The preparation method of embodiment 2-9 and embodiment 1 is similar, and the masterplate molecule that adopts when just preparing is different with the content of linking agent, and concrete outcome is seen table 1.
Table 1 separating effect
| Embodiment | Function monomer (mmol) | Template molecule (mmol) | Linking agent (mmol) | Selectivity factor α |
| 1 | 4 | 1 | 25 | 1.28 |
| 2 | 1 | 1 | 25 | 1.25 |
| 3 | 2 | 1 | 25 | 1.27 |
| 4 | 6 | 1 | 25 | 1.98 |
| 5 | 8 | 1 | 25 | 1.56 |
| 6 | 6 | 1 | 5 | 1.88 |
| 7 | 6 | 1 | 10 | 1.92 |
| 8 | 6 | 1 | 15 | 2.10 |
| 9 | 6 | 1 | 20 | 2.32 |
Claims (9)
1. the preparation method of a Yohimbine molecularly imprinted polymer is characterized in that: may further comprise the steps:
Function monomer methylacrylic acid and template molecule Yohimbine are dissolved in the methyl-sulphoxide, mixed at room temperature 6-24 hour, add linking agent TGM 1 and initiator then; Ultrasonic degas; Logical nitrogen deoxygenation, sealing back thermal-initiated polymerization is cleaned and is removed template molecule.
2. method as claimed in claim 2 is characterized in that: the mol ratio of template molecule and function monomer is: 1: 1-10, preferred 1: 1-8, more preferably 1: 4-8, most preferably 1: 6.
3. according to claim 1 or claim 2 method, it is characterized in that: the mol ratio of template molecule and linking agent is: 1: 5-30, preferred 1: 10-25, most preferably 1: 20.
4. method as claimed in claim 3 is characterized in that: the mol ratio of function monomer, template molecule and linking agent is: 6: 1: 20.
5. method as claimed in claim 4 is characterized in that: at least 5 minutes ultrasonic degas time.
6. method as claimed in claim 5 is characterized in that: at least 5 minutes oxygen deoxygenation time.
7. method as claimed in claim 6 is characterized in that: adopt the mixing solutions cleaning of methyl alcohol and acetate to remove template molecule.
8. method as claimed in claim 7 is characterized in that: the volume ratio of methyl alcohol and acetate is 1: 9.
9. Yohimbine molecularly imprinted polymer, it adopts each method preparation of claim 1-8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110331067XA CN102443101A (en) | 2011-10-27 | 2011-10-27 | Yohimbine detection material prepared by utilizing methacrylic acid and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110331067XA CN102443101A (en) | 2011-10-27 | 2011-10-27 | Yohimbine detection material prepared by utilizing methacrylic acid and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102443101A true CN102443101A (en) | 2012-05-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201110331067XA Pending CN102443101A (en) | 2011-10-27 | 2011-10-27 | Yohimbine detection material prepared by utilizing methacrylic acid and preparation method thereof |
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| CN (1) | CN102443101A (en) |
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- 2011-10-27 CN CN201110331067XA patent/CN102443101A/en active Pending
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Application publication date: 20120509 |