CN103285791B - A kind of based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons and its preparation method and application - Google Patents
A kind of based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons and its preparation method and application Download PDFInfo
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- CN103285791B CN103285791B CN201310172951.2A CN201310172951A CN103285791B CN 103285791 B CN103285791 B CN 103285791B CN 201310172951 A CN201310172951 A CN 201310172951A CN 103285791 B CN103285791 B CN 103285791B
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Abstract
The present invention relates to technical field of function materials, disclose a kind of preparation method based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons, comprise the following steps: 1) prepare magnetic particle with Iron(III) chloride hexahydrate; 2) magnetic particle is utilized to prepare particle dispersion; 3) in particle dispersion, add the ethanolic solution containing silester and tetrabutyl titanate, ultrasonic, stir, Magneto separate, remove template molecule, obtaining magnetic particle is core, SiO
2for the magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons of shell.Utilize method described in the application to prepare based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons can from the biological sample of complexity enrichment and purified polypeptide and low-molecular-weight albumen.Utilize the magnetic of affinitive material, greatly simplify complicated low abundance polypeptide and LMWP Sample Purification on Single and the process be separated, shorten the operating time.
Description
Technical field
The present invention relates to field of functional materials, invent a kind of based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons and preparation method thereof and application thereof.
Background technology
Having the biomolecule such as Inner source peptide, albumen of many small-molecular-weight in human body fluid, is some diseases Producing reason, is also result simultaneously.Detect the biomolecule of these small-molecular-weight, have very important effect to medical diagnosis on disease.
Mass spectrum is a kind of effective tool of detection biomolecule (particularly polypeptide and albumen) that can be quick, sensitive.Because in some samples, target peptide section concentration is low especially, containing high salt concentration or other nontarget organism molecule, and Mass Spectrometer Method is caused to carry out.Therefore, before Mass Spectrometer Method, need to these low-molecular-weight polypeptide or albumen is separated efficiently, enrichment, desalination and removal of impurities process, to improve the relative amount of tested substance.
Adopt the method for freeze-drying or evaporation and concentration sample, the relative concentration of sample can be improved, but due to the concentration also corresponding increase of salinity, and be difficult to avoid the interference to Mass Spectrometer Method; Conventional desalination way is the SiO adopting hydrophobic alkyl chain to modify
2filler, absorption polypeptide and albumen and reach purifying object, but for some complex samples containing a large amount of high abundance non-targeted albumen, but desalting ability is limited.In recent years, bibliographical information is also had to utilize mesoporous SiO
2duct volume exclusion effect purified polypeptide, but only rely on the effect of surface hydrophilic group silanol hydroxyl and polypeptide due to it, therefore limited to the affine accumulation ability of polypeptide.In addition, utilize these material enrichment polypeptide and albumen, often need centrifugation repeatedly, process complexity is loaded down with trivial details, and loss amount is large.
Summary of the invention
The object of the present invention is to provide a kind of based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons.
Second object is to provide a kind of preparation method based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons.
3rd object is to provide the application based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons, especially in the application of enrichment and purifying low molecular weight polypeptide and albumen from the biological sample of complexity.
For achieving the above object, concrete technical scheme is:
Based on a preparation method for metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons, comprise the following steps:
1) magnetic particle is prepared with Iron(III) chloride hexahydrate;
2) magnetic particle is utilized to prepare particle dispersion;
3) in particle dispersion, add the ethanolic solution containing silester and tetrabutyl titanate, ultrasonic, stir, Magneto separate, remove template molecule, obtaining magnetic particle is core, SiO
2for the magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons of shell.
Described magnetic particle is Fe
3o
4or Fe
2o
3.
Described step 2) be specially: get Fe
3o
4particle dispersion, in ethanol water, adds ammoniacal liquor, then adds template molecule, is uniformly dispersed, and obtains Fe
3o
4particle dispersion.
Described template molecule is cetyl ammonium bromide or cetyl chloride ammonium.
Described step 2) be specially: get 100mgFe
3o
4particle, is scattered in ethanol water water (water: alcohol=2:1), add 1 ?10mL ammoniacal liquor, add 600mg cetyl ammonium bromide, be uniformly dispersed, obtain Fe
3o
4particle dispersion.
Calcination method or organic solvent extractionprocess is adopted to remove template molecule in described step 3).
Described step 3) be specially get 0.25 ?1.25mL silester and 10-60 μ L tetrabutyl titanate be dissolved in 4mL ethanol, add Fe
3o
4in particle dispersion, stirring at room temperature 2h; Be warming up to 70 DEG C afterwards, continue to stir 6h; Magneto separate, ethanol washing is limpid to supernatant for several times; 80 DEG C of dried in vacuo overnight; Alcohol reflux washs more than 3 times or 550 DEG C of calcinings, obtains based on metal ion-modified magnetic mesoporous SiO
2nucleocapsid structure compatible micro balloons.
Based on a metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons, by magnetic core be modified with metal ion mesoporous silicon oxide shell and form, described magnetic core is Fe
3o
4magnetic particle.
By said method prepare based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons.
Described based on the metal ion-modified application of magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons in selective enrichment and purifying low molecular weight polypeptide and albumen.
Method described in the application by Metal Ions Modification to magnetic mesoporous SiO
2on, utilize the interaction of metal ion and polypeptide, affine polypeptide, also can utilize mesoporous volume exclusion effect simultaneously, remove a large amount of high-abundance proteins, and reach the object of enrichment and purifying, prepared based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons can from the biological sample of complexity enrichment and purified polypeptide and low-molecular-weight albumen.In addition, utilize the magnetic of affinitive material, greatly simplify Sample Purification on Single and separation process, shorten the operating time.
figure of description
Fig. 1: magnetic mesoporous SiO
2the TEM picture of compatible micro balloons;
Fig. 2: magnetic mesoporous SiO
2energy dispersive spectrometry (EDS) collection of illustrative plates of compatible micro balloons;
Fig. 3 A: the direct Mass Spectrometer Method of low concentration reference polypeptide, MALDI ?TOFMS figure;
Fig. 3 B: low concentration reference polypeptide is at magnetic mesoporous SiO
2mass Spectrometer Method after compatible micro balloons enrichment, MALDI ?TOFMS figure;
Fig. 4 A: the direct Mass Spectrometer Method of complicated polypeptide sample, MALDI ?TOFMS figure;
Fig. 4 B: complicated polypeptide sample is at magnetic mesoporous SiO
2mass Spectrometer Method after compatible micro balloons enriching and purifying, MALDI ?TOFMS figure.
Detailed description of the invention
Embodiment 1 is based on the preparation of metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons
1.Fe
3o
4prepared by magnetic particle
Prepared by employing solvent-thermal method, concrete steps are as follows: the Iron(III) chloride hexahydrate (FeC1 taking 5.13g
36H
2o) be distributed to equably in 80mL ethylene glycol and make solution, and add Surfactant PEG 1.25g and anhydrous sodium acetate 5.00g under magnetic stirring successively, stir into homogeneous system.This mixture is transferred in the 120mL autoclave with polytetrafluoroethylene (PTFE) lining and seals, finally autoclave is placed in insulating box and is heated to 200 DEG C and isothermal reaction 6h.After question response system cools naturally, gained suspension Magneto separate is obtained the powdered substance of black.Alternately wash several times with deionized water and ethanol again, in 60 DEG C of dry 8h, finally obtain Fe
3o
4particle product.
2. based on metal ion-modified magnetic mesoporous SiO
2prepared by nucleocapsid structure compatible micro balloons
Concrete steps are as follows: 100mgFe
3o
4particle, is scattered in ethanol water (water: alcohol=2:1), adds 2.4mL ammoniacal liquor, add 600mgCTAB cetyl ammonium bromide (template molecule), be uniformly dispersed, obtain Fe
3o
4particle dispersion;
Get 500 μ L silester (TEOS) and be dissolved in 4mL ethanol (Si:Ti=10:1) with 50 μ L tetrabutyl titanates, after shaken well, slowly add Fe
3o
4in particle dispersion, stirring at room temperature 2h; Be warming up to 70 DEG C afterwards, continue to stir 6h; Magneto separate, ethanol washing is limpid to supernatant for several times; 80 DEG C of dried in vacuo overnight; Alcohol reflux washs more than 3 times or 550 DEG C of calcinings, obtains based on metal ion-modified magnetic mesoporous SiO
2nucleocapsid structure compatible micro balloons, its transmission electron microscope photo as shown in Figure 1.Can observe from Fig. 1, prepared compatible micro balloons has obvious nucleocapsid structure, outer shell can be observed obvious short-track mesoporous.Its energy dispersive spectrometry (EDS) collection of illustrative plates as shown in Figure 2.Prepared compatible micro balloons is made up of Fe, O, Si and Ti tetra-kinds of elements.Above result proves, embodiment 1 has successfully prepared metal ion-modified magnetic mesoporous SiO
2nucleocapsid structure compatible micro balloons.
Embodiment 2 utilizes based on the metal ion-modified low abundance standard peptide of magnetic mesoporous SiO2 nucleocapsid structure compatible micro balloons enrichment
1. the preparation of sample solution: the improvement on synthesis MW=1533.6 solution of preparation 50mL5nM.
2. the enrichment of improvement on synthesis and mass spectral analysis: get 500 μ L aforementioned polypeptides solution, add the magnetic mesoporous SiO of 100ug
2compatible micro balloons, is uniformly dispersed, vibration 10min.Remove supernatant after Magneto separate, 5 μ L80% acrylonitrile (CAN), 0.5% trifluoroacetic acid (TFA) (v/v), vibrate after 5 minutes, Magneto separate.Collect supernatant, get 0.7uL sample, mix with 0.7 matrix, put on MALDI-TOF target plate, form cocrystallization, carry out mass spectral analysis.
3. analysis result: Fig. 3 A is before the enrichment of 5nM reference polypeptide, directly carries out the result of Mass Spectrometer Method.Because peptide concentration is very low, so be difficult to effective mass signal be detected.Fig. 3 B is that 5nM reference polypeptide is through metal ion-modified magnetic mesoporous SiO
2the mass spectrogram detected is carried out again after compatible micro balloons enrichment.Can observe, after enrichment, signal strength signal intensity and the signal to noise ratio of reference polypeptide all improve a lot.From Fig. 3 A and Fig. 3 B, metal ion-modified magnetic mesoporous SiO
2the reference polypeptide of compatible micro balloons to low concentration has good concentration effect.
Embodiment 3 utilizes based on metal ion-modified magnetic mesoporous SiO
2low abundance peptide in nucleocapsid structure compatible micro balloons enrichment complex sample
1. the preparation of sample solution: the bovine serum albumin(BSA) BSA taking lmg is dissolved in the Ammonium bicarbonate food grade solution of lmL50mM (pH8.0), trypsin digestion is added 16 hours according to the ratio with tryptic mass ratio 50:1, hydrolysis temperature controls at 37 DEG C, finally adds 1% formic acid cessation reaction.Get 50uL polypeptide solution, be diluted to 5nM with the aqueous solution containing 4M urea, for subsequent use.
2. the enrichment of polypeptide and mass spectral analysis: get 500uL aforementioned polypeptides solution, add the magnetic mesoporous SiO of 100ug
2compatible micro balloons, is uniformly dispersed, vibration 10min.Remove supernatant after Magneto separate, use 500uL deionized water, washing compatible micro balloons, Magneto separate, removes supernatant, repeats twice; Add 5 μ L80%ACN, 0.5%TFA (v/v) washings, vibrate after 5 minutes, Magneto separate.Collect supernatant, get 0.7uL sample, mix with 0.7 matrix, put on MALDI-TOF target plate, form cocrystallization, carry out mass spectral analysis.
3. analysis result: Fig. 4 A is before 5nMBSA proteolytic cleavage liquid enrichment, directly carries out the result of Mass Spectrometer Method.Because peptide concentration is very low, and there is the interference of the pollutants such as a large amount of salt, so the intensity of mass signal and signal to noise ratio are all very low, 4 polypeptide peak belonging to BSA albumen only can be detected.Fig. 4 B is that 5nMBSA proteolytic cleavage liquid is through metal ion-modified magnetic mesoporous SiO
2the mass spectrogram detected is carried out again after compatible micro balloons enrichment.Can observe, after enrichment, signal strength signal intensity and the signal to noise ratio of reference polypeptide all improve a lot, and 44 polypeptide peak belonging to BSA albumen can be detected.From Fig. 4 A and Fig. 4 B, magnetic mesoporous SiO
2the mixed polypeptide of compatible micro balloons to the low concentration containing high salt concentration has good concentration effect.The polypeptide of table 1 for detecting in mixed polypeptide solution and identifying.
The polypeptide that table 1 detects and identifies in mixed polypeptide solution
| Position in BSA albumen | Theoretical molecular | Peptide sequence |
| 29–34 | 711.3664 | K.SEIAHR.F |
| 35–44 | 1248.614 | R.FKDLGEEHFK.G |
| 37–44 | 973.4505 | K.DLGEEHFK.G |
| 66–75 | 1162.623 | K.LVNELTEFAK.T |
| 89–100 | 1361.665 | K.SLHTLFGDELCK.V |
| 123–130 | 976.4436 | R.NECFLSHK.D |
| 131–138 | 885.408 | K.DDSPDLPK.L |
| 139–151 | 1518.739 | K.LKPDPNTLCDEFK.A |
| 139–155 | 1961.94 | K.LKPDPNTLCDEFKADEK.K |
| 161–167 | 926.4861 | K.YLYEIAR.R |
| 168–183 | 2044.021 | R.RHPYFYAPELLYYANK.Y |
| 169–183 | 1887.92 | R.HPYFYAPELLYYANK.Y |
| 198–204 | 700.3942 | K.GACLLPK.I |
| 212–218 | 702.4024 | K.VLASSAR.Q |
| 229–235 | 819.4603 | K.FGERALK.A |
| 229–235 | 819.4603 | K.FGERALK.A |
| 233–241 | 1000.582 | R.ALKAWSVAR.L |
| 242–248 | 846.4963 | R.LSQKFPK.A |
| 246–256 | 1293.697 | K.FPKAEFVEVTK.L |
| 286–297 | 1385.613 | K.YICDNQDTISSK.L |
| 298–309 | 1417.731 | K.LKECCDKPLLEK.S |
| 310–318 | 1014.48 | K.SHCIAEVEK.D |
| 341–346 | 751.35 | K.NYQEAK.D |
| 347–359 | 1566.735 | K.DAFLGSFLYEYSR.R |
| 360–371 | 1438.805 | R.RHPEYAVSVLLR.L |
| 361–371 | 1282.703 | R.HPEYAVSVLLR.L |
| 402–412 | 1304.709 | K.HLVDEPQNLIK.Q |
| 413–420 | 1010.413 | K.QNCDQFEK.L |
| 421–433 | 1478.788 | K.LGEYGFQNALIVR.Y |
| 437–451 | 1638.931 | R.KVPQVSTPTLVEVSR.S |
| 438–451 | 1510.836 | K.VPQVSTPTLVEVSR.S |
| 452–459 | 816.4818 | R.SLGKVGTR.C |
| 456–468 | 1464.681 | K.VGTRCCTKPESER.M |
| 460–468 | 1051.443 | R.CCTKPESER.M |
| 469–482 | 1666.806 | R.MPCTEDYLSLILNR.L |
| 483–489 | 840.4527 | R.LCVLHEK.T |
| 499–507 | 1023.448 | K.CCTESLVNR.R |
| 508–523 | 1822.892 | R.RPCFSALTPDETYVPK.A |
| 548–557 | 1141.707 | K.KQTALVELLK.H |
| 549–557 | 1013.612 | K.QTALVELLK.H |
| 562–568 | 817.4181 | K.ATEEQLK.T |
| 569–580 | 1398.685 | K.TVMENFVAFVDK.C |
| 588–597 | 1049.485 | K.EACFAVEGPK.L |
| 598–607 | 1001.576 | K.LVVSTQTALA.- |
Claims (10)
1., based on a preparation method for metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons, comprise the following steps:
1) magnetic particle is prepared with Iron(III) chloride hexahydrate;
2) magnetic particle is utilized to prepare the particle dispersion containing template molecule;
3) in particle dispersion, add the ethanolic solution containing silester and tetrabutyl titanate, ultrasonic, heat up after stirring at room temperature again and continue to stir, Magneto separate, remove template molecule, obtaining magnetic particle is core, metal ion-modified SiO
2for the magnetic mesoporous nucleocapsid structure compatible micro balloons of shell.
2. a kind of preparation method based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons according to claim 1, it is characterized in that, described magnetic particle is Fe
3o
4or Fe
2o
3.
3. a kind of preparation method based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons according to claim 1, it is characterized in that, described magnetic particle is Fe
3o
4particle, described step 2) be specially: get magnetic particle and be scattered in ethanol water, add ammoniacal liquor, then add template molecule, ultrasonic disperse, obtain Fe
3o
4particle dispersion.
4. a kind of preparation method based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons according to claim 3, it is characterized in that, described template molecule is cetyl ammonium bromide or cetyl chloride ammonium.
5. a kind of preparation method based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons according to claim 3, is characterized in that, described step 2) be specially: get 100mgFe
3o
4particle, be scattered in the solution of 160ml deionized water and 80mL ethanol composition, add 2.4mL ammoniacal liquor, add 600mg cetyl ammonium bromide, ultrasonic disperse 30min, obtains Fe
3o
4particle dispersion.
6. a kind of preparation method based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons according to claim 1, is characterized in that, described step 3) in adopt calcination method or organic solvent extractionprocess to remove template molecule.
7. a kind of preparation method based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons according to claim 6, it is characterized in that, described step 3) be specially and get 428uL silester and 32.8uL tetrabutyl titanate is dissolved in 4mL ethanol, after shaken well, slowly add step 2) in preparation particle dispersion in, after ultrasonic 10min, stirring at room temperature 2h; Be warming up to 70 DEG C afterwards, continue to stir 6h; Magneto separate, ethanol washing is limpid to supernatant for several times; 80 DEG C of dried in vacuo overnight; 550 DEG C of calcinings, burn off template molecule obtains based on metal ion-modified magnetic mesoporous SiO
2nucleocapsid structure compatible micro balloons.
8., based on a metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons, by magnetic core be modified with metal ion mesoporous silicon oxide shell and form, described magnetic core is Fe
3o
4magnetic particle.
9. by method described in claim 1-7 any one prepare based on metal ion-modified magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons.
10. described in claim 8 or 9 based on the metal ion-modified application of magnetic mesoporous silicon dixoide nucleocapsid structure compatible micro balloons in selective enrichment and purifying low molecular weight polypeptide and albumen.
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| CN105982337A (en) * | 2016-05-13 | 2016-10-05 | 浙江省海洋开发研究院 | Aquatic collagen peptide food used for adjuvant therapy of osteoporosis and arthritis |
| CN105982331A (en) * | 2016-05-13 | 2016-10-05 | 浙江省海洋开发研究院 | Universal type aquatic collagen peptide food for wound healing |
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| CN114956721B (en) * | 2022-05-06 | 2023-05-23 | 山西中科赛德能源科技有限公司 | High-strength superfine deep hole grouting reinforcement material and preparation method thereof |
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