CN103592290A - Analysis method for quantitative characterization on functional gold nano-particle hydrophobicity intensity - Google Patents
Analysis method for quantitative characterization on functional gold nano-particle hydrophobicity intensity Download PDFInfo
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Abstract
The invention discloses an analysis method for quantitative characterization on functional gold nano-particle hydrophobicity intensity. The analysis method comprises the following steps of preparing a water-saturated n-octanol solution and an n-octanol-saturated aqueous solution, adding gold nano-particles to be determined into the n-octanol-saturated aqueous solution, carrying out uniform mixing, adding the water-saturated n-octanol solution into the mixed solution, carrying out vibration and then standing to obtain an oil-water two-phase solution, respectively taking the same volumes of the oil phase and the water phase solutions, adding them into a colorimetric tube, carrying out drying until the solvent completely volatilizes, adding aqua regia into the colorimetric tube for digestion, carrying out volume metering by high-purity water so that sample solution acidity is less than 10%, detecting Au content of the sample solution by ICP-AES or ICP-MS, and calculating a gold nano-particle lipo-hydro partition coefficient log P according to a formula of Log P=Log(Co/Cw). The analysis method realizes quantitative characterization on functional gold nano-particle hydrophobicity intensity. The analysis method has simple, easy, stable and reliable processes, saves time and labor and can be widely used for determination on nano-material hydrophobicity intensity.
Description
Technical field
The present invention relates to a kind of analytical approach of quantitatively characterizing nano material hydrophobicity intensity, relate in particular to a kind of analytical approach of quantitatively characterizing functionalization gold nano grain material hydrophobicity intensity.
Background technology
Nano material has the ability through biological barriers such as cell membranes, is widely used in a plurality of biomedical aspects such as target carrying medicine, biological developing, medical diagnosis on disease and gene therapy.When nano material enters physiological environment (as blood, tissue fluid and tenuigenin), nano material inevitably can interact with biomolecule such as protein.Both interactional results not only likely affect the 26S Proteasome Structure and Function of protein, also will directly affect nano material kinetic property and the biologically active under physiological environment in vivo.And the surface chemical property of nano material can affect biomolecule (as protein) and its interaction, thereby affect its biologically active.Surface hydrophilic and hydrophobic is one of of paramount importance surface properties of nano material, and its change can affect or control nano material by the interaction of hydrophobic effect and biomolecule.For the water-soluble and biocompatibility of nano material is improved, conventionally at nano-material surface, introduce functionalization chemical group.For example, protein molecule has higher affinity to nano particle hydrophobic surface, and the size of affinity not only determines kind and the quantity of adhesion protein, and the degree also changing with protein structure has certain relation.In existing research, to nano-material surface, the ratio of hydrophobic grouping in reaction ratio is normally controlled in hydrophobic change, and lacks quantification criterion to modifying the surface hydrophobic of rear nano material.Based on this, particularly important to the hydrophobic analysis of nano-material surface.
By OCA15 optics contact angle tester, measure the contact angle of material surface, can qualitatively draw the hydrophobicity of material, but utilize the measurement of functionalized nano material lipid log P to come the analytical approach of the hydrophobicity intensity of this material of quantitatively characterizing have not been reported through retrieval.
Summary of the invention
For the deficiency of the contact angle method of OCA15 optics contact angle tester qualitative determination material surface, the object of the present invention is to provide a kind of analytical approach of quantitatively characterizing functionalization gold nano grain hydrophobicity intensity.
The analytical approach of quantitatively characterizing functionalization gold nano grain material hydrophobicity intensity of the present invention, step is:
1) isopyknic high purity water and the pure n-octyl alcohol of top grade are mixed, and stir 24～30h, then standing, after solution layering, present oil phase and the water of obvious separation, upper strata is water saturated n-octyl alcohol solution, lower floor is the aqueous solution that n-octyl alcohol is saturated, collects respectively two phase liquid and saves backup;
2) getting gold nano grain material to be determined is added in graduated centrifuge tube, add the aqueous solution that n-octyl alcohol is saturated, after mixing, then add the water saturated n-octyl alcohol solution with aqueous solution same volume, with sealed membrane, seal the centrifugal mouth of pipe, put jolting 24～30h under 25 ± 1 ℃ of conditions;
3) centrifuge tube after jolting is standing, wait manage interior oil phase and aqueous phase separation boundary line clear after, take out respectively two phase liquid and go in new centrifuge tube;
4) get respectively oil phase and the aqueous phase solution of the step 3) collection of same volume, be added in 10mL color comparison tube, 120 ℃ of vacuum drying to solvents volatilize completely;
5) in the dried color comparison tube of step 4), add 250 μ L～500 μ L new system chloroazotic acid, clear up 12～30h, then with high purity water, be settled to 5mL～10mL, and to make sample solution acidity be 5%～10%;
6) according to the concentration range of setting, prepare the goldstandard solution of a series of concentration, and make solution acidity keep consistent with step 5) sample solution acidity;
7) with the quantitative detecting step 5 of ICP-AES (ICP-AES) or inductively coupled plasma mass spectrometry (ICP-MS)) in each sample solution be the content of Au element in oil phase and water, according to formula Log P=Log (Co/Cw), calculate the value of the lipid log P of gold nano, wherein Co and Cw are respectively the concentration of nano material in n-octyl alcohol and water, can realize the hydrophobicity intensity of the gold nano grain material of quantitatively characterizing mensuration according to concrete log P value.
In the analytical approach of above-mentioned quantitatively characterizing functionalization gold nano grain material hydrophobicity intensity: step 2), mix that preferred employing is ultrasonic to be mixed, particularly disperse bad gold nano-material can be before adding water saturated n-octyl alcohol solution ultrasonic mixing.
In the analytical approach of above-mentioned quantitatively characterizing functionalization gold nano grain material hydrophobicity intensity: the to be determined gold nano grain concentration of the uptake of oil phase and aqueous phase solution depending on containing in its solution described in step 4), concentration height is got less, low get of concentration more, but uptake is no more than 10mL.
In the analytical approach of above-mentioned quantitatively characterizing functionalization gold nano grain material hydrophobicity intensity: described in step 4), oil phase and aqueous phase solution, when adding color comparison tube, do not touch tube wall as far as possible, particularly top tube wall, prevent chloroazotic acid clear up less than.
In the analytical approach of above-mentioned quantitatively characterizing functionalization gold nano grain material hydrophobicity intensity: described in step 7) with the quantitative detecting step 5 of ICP-AES (ICP-AES) or inductively coupled plasma mass spectrometry (ICP-MS)) in each sample solution be the content of Au element in oil phase and water, adopt 3 parallel experiments, calculate the content that its mean value obtains Au element.
The present invention has following beneficial effect:
I) medicine used herein, instrument and instrument are the common object in laboratory, and method step is simple and easy to do, reliable and stable, time saving and energy saving.
2) the present invention can quantitatively characterizing material hydrophobicity intensity, can be widely used in the mensuration of nano material hydrophobicity intensity.
Accompanying drawing explanation
Fig. 1: surface hydrophobic changes the TEM figure of gold nano 7 kinds of gold nano grains of series (GNP-1 to GNP-7) continuously
Wherein:
A: be the picture of GNP-1 under transmission electron microscope; Its medium scale is 50nm,
B: be the picture of GNP-2 under transmission electron microscope; Its medium scale is 50nm,
C: be the picture of GNP-3 under transmission electron microscope; Its medium scale is 50nm,
D: be the picture of GNP-4 under transmission electron microscope; Its medium scale is 50nm,
E: be the picture of GNP-5 under transmission electron microscope; Its medium scale is 50nm,
F: be the picture of GNP-6 under transmission electron microscope; Its medium scale is 50nm,
G: be the picture of GNP-7 under transmission electron microscope; Its medium scale is 50nm.
Fig. 2: 7 kinds of gold nano grains are at the distribution Visual Graph of profit two-phase.
Fig. 3: this method is measured the result of the resulting log P of 7 kinds of gold nano grains (GNP-1 to GNP-7).
Embodiment
7 kinds of surface hydrophobics change the synthetic of gold nano grain
The present invention utilizes sodium borohydride reduction to prepare gold nano, first with sodium borohydride, gold chloride is reduced into gold nano, five-membered ring in the part of two kinds of lipoic acid derivatives is opened simultaneously, by Au-S key, is connected with gold nano surface, and reaction equation is as follows.Selected two kinds of ligand Ligand-1 and Ligand-2 have respectively stronger hydrophobicity and water wettability, thereby obtain by the different mixing proportion that the former two is reacted in control the functionalization gold nano grain that hydrophobicity is different.
Concrete operation step is as follows:
1. accurately measure the 20mg/mL HAuCl of 0.625mL
44H
2o aqueous solution in 100mL round-bottomed flask, add 6mL to be dissolved with different proportion Ligand-1 and Ligand-2(as shown in table 1) DMF (DMF) solution, under room temperature condition, stir.
After 2.30min, slowly dropwise splash into 6mL NaBH
4(5.0mg, 0.131mmol), solution has become redness at once, and after dropwising, reaction normal temperature continues reaction 4h.
3., after reaction finishes, the centrifugal supernatant that goes of reactant liquor is removed to excessive ligand, and add DMF:H
2o(1:1) solution is again after ultrasonic dispersion, more centrifugal, repeats to use DMF:H
2o(1:1) after solution washing 4-5 time, use intermediate water washed twice, GNPs is dispersed in the intermediate water of about 5mL the most at last, makes the concentration of Au in solution about 1mg/mL.Obtain respectively 7 kinds of gold nano grains (GNP-1 to GNP-7).
4.ICP-AES or ICP-MS measure Au concentration.
Table 1: complex functionality gold nano grain adds the quality of two kinds of ligands
With transmission electron microscope (TEM), the gold nano grain obtaining in embodiment 1 is carried out to morphology analysis:
On copper mesh, drip respectively (7 kinds: GNP-1 to GNP-7) sample solution of the gold nano grains of 10 μ L, (water sample) or 120 ℃ of vacuum drying 2h(n-octyl alcohol samples dry half an hour under infrared lamp more than) after, utilize the low resolution transmission electron microscope of JEM-1011 to measure.As shown in Figure 1, gold nano grain is sub-circular to the gold nano grain pattern of observing, and mean grain size is in 5 nanometer left and right.
The determination step of gold nano grain lipid is as follows:
1) isopyknic high purity water and the pure n-octyl alcohol of top grade are mixed, and stir 24h, then standing, after solution layering, present oil phase and the water of obvious separation, upper strata is water saturated n-octyl alcohol solution, lower floor is the aqueous solution that n-octyl alcohol is saturated, collects respectively two phase liquid and saves backup;
2) get respectively 7 kinds of the GNPs(gold nano grain materials of 0.3mg: GNP-1 to GNP-7) be added in 5mL graduated centrifuge tube, add the aqueous solution 1mL that n-octyl alcohol is saturated, after mixing (disperse bad gold nano-material can before adding n-octyl alcohol ultrasonic mixing), add again the water saturated n-octyl alcohol solution with aqueous solution same volume, with sealed membrane, seal the centrifugal mouth of pipe, put jolting 24 under 25 ± 1 ℃ of conditions;
3) centrifuge tube after jolting is standing, wait to manage behind interior oil phase and aqueous phase separation boundary line clear (about 0.5-1.0h can shorten the time for the nano material of free settling), with liquid-transfering gun, take out respectively two phase liquid and go in new centrifuge tube;
4) (uptake is depending on gold nano grain concentration to get respectively oil phase that the step 3) of same volume collects and aqueous phase solution, be generally 5mL), be added in 10mL color comparison tube and (try one's best not rebuffed, particularly the tube wall of top, prevent from clearing up less than), 120 ℃ of vacuum drying to solvents volatilize completely;
5) in the dried color comparison tube of step 4), add 500 μ L new system chloroazotic acid, clear up 20h, if be then settled to 10mL(gold nano grain concentration when lower with high purity water, can add 250 μ L chloroazotic acid and clear up, be settled to 5mL), and to make sample solution acidity be 5%;
6) according to the concentration range of setting, prepare the goldstandard solution of a series of concentration, and make solution acidity keep consistent with step 5) sample solution acidity;
7) with the quantitative detecting step 5 of ICP-AES (ICP-AES) or inductively coupled plasma mass spectrometry (ICP-MS)) in each sample solution be the content (3 parallel experiment mean value) of Au element in oil phase and water, according to formula Log P=Log (Co/Cw), calculate the value of the lipid log P of gold nano, wherein Co and Cw are respectively the concentration of nano material in n-octyl alcohol and water, can realize the hydrophobicity intensity of the gold nano grain material of quantitatively characterizing mensuration according to concrete log P value.The results are shown in Figure 3.
Claims (5)
1. an analytical approach for quantitatively characterizing functionalization gold nano grain material hydrophobicity intensity, step is:
1) isopyknic high purity water and the pure n-octyl alcohol of top grade are mixed, and stir 24～30h, then standing, after solution layering, present oil phase and the water of obvious separation, upper strata is water saturated n-octyl alcohol solution, lower floor is the aqueous solution that n-octyl alcohol is saturated, collects respectively two phase liquid and saves backup;
2) getting gold nano grain material to be determined is added in graduated centrifuge tube, add the aqueous solution that n-octyl alcohol is saturated, after mixing, then add the water saturated n-octyl alcohol solution with aqueous solution same volume, with sealed membrane, seal the centrifugal mouth of pipe, put jolting 24～30h under 25 ± 1 ℃ of conditions;
3) centrifuge tube after jolting is standing, wait manage interior oil phase and aqueous phase separation boundary line clear after, take out respectively two phase liquid and go in new centrifuge tube;
4) get respectively oil phase and the aqueous phase solution of the step 3) collection of same volume, be added in 10mL color comparison tube, 120 ℃ of vacuum drying to solvents volatilize completely;
5) in the dried color comparison tube of step 4), add 250 μ L～500 μ L new system chloroazotic acid, clear up 12～30h, then with high purity water, be settled to 5mL～10mL, and to make sample solution acidity be 5%～10%;
6) according to the concentration range of setting, prepare the goldstandard solution of a series of concentration, and make solution acidity keep consistent with step 5) sample solution acidity;
7) with the quantitative detecting step 5 of ICP-AES (ICP-AES) or inductively coupled plasma mass spectrometry (ICP-MS)) in each sample solution be the content of Au element in oil phase and water, according to formula Log P=Log (Co/Cw), calculate the value of the lipid log P of gold nano, wherein Co and Cw are respectively the concentration of nano material in n-octyl alcohol and water, can realize the hydrophobicity intensity of the gold nano grain material of quantitatively characterizing mensuration according to concrete log P value.
2. the analytical approach of quantitatively characterizing functionalization gold nano grain material hydrophobicity intensity according to claim 1, is characterized in that: step 2) described in mix and adopt ultrasonic mixing.
3. the analytical approach of quantitatively characterizing functionalization gold nano grain material hydrophobicity intensity according to claim 1, it is characterized in that: the to be determined gold nano grain concentration of the uptake of oil phase and aqueous phase solution depending on containing in its solution described in step 4), concentration height is got less, low get of concentration more, but uptake is no more than 10mL.
4. the analytical approach of quantitatively characterizing functionalization gold nano grain material hydrophobicity intensity according to claim 1, it is characterized in that: described in step 4), oil phase and aqueous phase solution are when adding color comparison tube, do not touch tube wall as far as possible, particularly top tube wall, prevent chloroazotic acid clear up less than.
5. the analytical approach of quantitatively characterizing functionalization gold nano grain material hydrophobicity intensity according to claim 1, it is characterized in that: described in step 7) with the quantitative detecting step 5 of ICP-AES (ICP-AES) or inductively coupled plasma mass spectrometry (ICP-MS)) in each sample solution be the content of Au element in oil phase and water, adopt 3 parallel experiments, calculate the content that its mean value obtains Au element.
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Cited By (5)
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| CN103979482A (en) * | 2014-04-25 | 2014-08-13 | 山东大学 | Gold nanoparticle array capable of removing perfluorinated pollutant |
| CN105535990A (en) * | 2016-01-08 | 2016-05-04 | 山东大学 | Spherical gold nanoparticle array with surface hydrophilic/hydrophobic property differentiated and application thereof |
| CN110672485A (en) * | 2019-09-06 | 2020-01-10 | 浙江大学 | Method for accurately measuring surface hydrophobicity of activated sludge by adsorbing dye |
| CN110672486A (en) * | 2019-09-06 | 2020-01-10 | 浙江大学 | Method for accurately measuring surface hydrophobicity of aerobic granular sludge by adsorbing phenanthrene |
| CN113646630A (en) * | 2019-03-29 | 2021-11-12 | 百时美施贵宝公司 | Method for measuring hydrophobicity of chromatographic resin |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103979482A (en) * | 2014-04-25 | 2014-08-13 | 山东大学 | Gold nanoparticle array capable of removing perfluorinated pollutant |
| CN105535990A (en) * | 2016-01-08 | 2016-05-04 | 山东大学 | Spherical gold nanoparticle array with surface hydrophilic/hydrophobic property differentiated and application thereof |
| CN113646630A (en) * | 2019-03-29 | 2021-11-12 | 百时美施贵宝公司 | Method for measuring hydrophobicity of chromatographic resin |
| CN113646630B (en) * | 2019-03-29 | 2024-05-07 | 百时美施贵宝公司 | Method for measuring hydrophobicity of chromatographic resin |
| CN110672485A (en) * | 2019-09-06 | 2020-01-10 | 浙江大学 | Method for accurately measuring surface hydrophobicity of activated sludge by adsorbing dye |
| CN110672486A (en) * | 2019-09-06 | 2020-01-10 | 浙江大学 | Method for accurately measuring surface hydrophobicity of aerobic granular sludge by adsorbing phenanthrene |
| CN110672485B (en) * | 2019-09-06 | 2020-07-28 | 浙江大学 | Method for accurately measuring surface hydrophobicity of activated sludge by adsorbing dye |
| CN110672486B (en) * | 2019-09-06 | 2020-08-18 | 浙江大学 | Method for accurately measuring surface hydrophobicity of aerobic granular sludge by adsorbing phenanthrene |
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Application publication date: 20140219 |