CN101268946A - Method for latency fingerprint appearance of surface functionalization nano-gold particle - Google Patents
Method for latency fingerprint appearance of surface functionalization nano-gold particle Download PDFInfo
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- CN101268946A CN101268946A CNA2008100506747A CN200810050674A CN101268946A CN 101268946 A CN101268946 A CN 101268946A CN A2008100506747 A CNA2008100506747 A CN A2008100506747A CN 200810050674 A CN200810050674 A CN 200810050674A CN 101268946 A CN101268946 A CN 101268946A
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Abstract
The invention belongs to the technical field of trace amount detection, in particular relates to a method that surfaces functionalized nanogold particles are used for potential fingerprint appearance. The invention provides the method that the different surface functionalized nanogold particles (probe) are used for the potential fingerprint appearance. The particles are the hydrophobixated nanogold particles decorated by alkyl hydrosulfide, the hydrophobixated nanogold particles protected by surface active agent cetane trimethyl ammonium bromide (CTAB), the water-soluble nanogold particles protected by the CTAB and the water-soluble nanogold particles protected by L-cysteine respectively. The probe and the ingredients in the residual sweat in the potential fingerprint generate the absorption and static functions or the condensation reaction, then an argentation is utilized to lead potential fingerprint samples to colorate in the argentation liquid, the nanogold particle signals for the ingredient identification in the fingerprint are magnified and the reduced argentum particles deposite at the grain position of the fingerprint samples to further present black, thereby forming the clear fingerprint image that can be observed by naked eyes. The method is simple, fast and high in sensitivity and has no harmful side effects.
Description
Technical field
The invention belongs to the trace detection technical field, be specifically related to surface-functionalized nanogold particle and be used for the latent fingerprint method for visualizing.
Background technology
It is variant that fingerprint has the people, throughout one's life constant and touch the characteristics of thing trace, therefore, plays important evidential function in the criminal suit process.Science correctly find, extract, manifest identify fingerprint for carry out investigation, punishing crime has important practice effect.Fingerprint identification is one of the most reliable method of carrying out individual identification, in forensic science, in the investigation of accident and handling, often can provide definite identification by taking the fingerprint.And along with popularizing and the application of automatic system of fingerprint recognition of computer technology, fingerprint technique and soon more and more widely used in people's life.
From 1877, Charles Robert Richet Aubert utilized silver nitrate to manifest since the sweat fingerprint in the paper delivery, and fingerprint manifestation has become the professional technique of subject knowledges such as an integrated use physics, chemistry, biology and technology.Being applied to on-the-spot biological trace method for visualizing at present mainly contains: optics appearance method, physics appearance method and chemical appearance method.The common weakness of these methods is that sensitivity is low, and sensitivity and result to DNA tests after the method that wherein has is used produce interference.Existingly manifest reagent and still there is hidden danger in process for show, as take to brush be suspended in airborne small grain size dust when showing method, some has the fluorescent dye and the smoked toxic and harmful that the substance decomposition reaction produces when showing method of carcinogenesis, they all cause serious harm to professional and technical personnel healthy.Present most widely used powder method, the deadly defect of this method are to manifest outmoded fingerprint.The development of novel gasifying agent is owing to be subjected to the restriction of safety and cost, also achieving no breakthrough property progress.The produced simultaneously background fluorescence of luminescence generated by light technology that uses is very big to the interference of the biological print identification of luminescence generated by light of routine at present, and difficulty reaches the requirement of expection.Therefore do not have the research and development that poison with the on-the-spot biological trace appearing technique of high sensitivity and become the emphasis of forensic science research and countries in the world Forensic Science personnel's striving direction.
For the organic components in the latent fingerprint, as oils and fats, aminoacid, vitamin etc., because quality too small (nanogram level), so under considerable situation, the process for show that requires to adopt should possess extra high sensitivity.The nanogold particle of functionalization can adsorb with oils, the amino acids material in the fingerprint, utilize the recognition function (and in conjunction with the recognition reaction between its functionalization group) of the dimensional effect combined function group of nano material, come that presentation time is more of a specified duration exactly, soaked or destructive fingerprint, thereby the fingerprint region that can manifest identification enlarges.
The present invention proposes to utilize the nanogold particle of functionalization in conjunction with argentation latent fingerprint to be carried out method for visualizing.
Summary of the invention
The purpose of this invention is to provide surface-functionalized nanogold particle and be used for the latent fingerprint method for visualizing, method is simple, quick, highly sensitive; The operator is had no side effect, not the latent fingerprint process for show that can realize by instrument.
The nanogold particle (probe 1, probe 2, probe 3, probe 4) that the invention provides the different surfaces functionalization is used for the latent fingerprint method for visualizing.Wherein, probe 1 is modified the nanogold particle of hydrophobization for alkyl hydrosulfide; Probe 2 is the nanogold particle of the hydrophobization of surfactant cetyl trimethyl ammonium bromide (CTAB) protection; Probe 3 is the water miscible nanogold particle of CTAB protection; Probe 4 is the water-soluble nano gold grain of L-cysteine protection.
The solution of the present invention is: surface-functionalized nanogold particle (probe 1, probe 2, probe 3, probe 4), adsorb with the composition in the residual perspiration in the latent fingerprint, electrostatic interaction or condensation reaction, utilize argentation then, the latent fingerprint sample is developed the color in silver-colored dye liquor, to amplify with the nanogold particle signal of composition identification in the fingerprint, thereby the silver-colored granule that is reduced presents black in the lines place of sample fingerprint deposition, observes fingerprint image clearly but form bore hole.
One, mercaptan modification gold nano grain is the preparation and the process for show of probe 1:
The preparation of probe 1: under the room temperature, the aqueous solution of chloraurate of 20～50mmol/L mixes with the toluene solution of 40～80mmol/L, four octyl group ammonium bromide and stirs, and phase transfer reagent four octyl group ammonium bromide are transferred to gold chloride in the organic facies toluene fully; In organic facies, add 12 or Stearyl mercaptan then; Follow violent stirring; join the sodium borohydride frozen water solution of 0.1～0.4mol/L of preparation newly in the mixed solution lentamente; after continuing to stir 2～3h organic facies is separated; rotary evaporation surplus solution under 30～50 ℃ of conditions; add ethanol then and be placed on-18～20 ℃ and leave standstill 2～4h, the atropurpureus that obtains precipitation is the gold nano grain (probe 1) of the alkyl hydrosulfide protection of hydrophobization.
Fingerprint manifestation method: at room temperature, with probe 1 by weight volume ratio 0.01～0.05% (w/v) concentration be distributed to and make gold colloidal in the petroleum ether, make the A4 pattern product that are printed on latent fingerprint behind water logging bubble 2～5min, put into gold colloidal and soak 5～15min, take out sample clear water rinsing, immerse then in the silver-colored dye liquor for preparing, (as 5min) takes out and dries after several minutes, and latent fingerprint manifests also and can directly observe by bore hole in the sample.
Two, the preparation and the fingerprint manifestation method of the gold colloidal of cetyl trimethyl ammonium bromide (CTAB) functionalization (probe 2, probe 3):
(1) gold colloidal of the hydrophobization of Surfactant CTAB modification is a probe 2: under the room temperature, 2mM cetyl trimethyl ammonium bromide toluene or chloroformic solution are mixed with 0.5～5% aqueous solution of chloraurate, behind vigorous stirring 2～5min, static layering is isolated organic layer as in another container; In remaining aqueous solution of chloraurate, add cetyl trimethyl ammonium bromide toluene or chloroformic solution again and still can make aqueous solution of chloraurate continue phase transfer to organic solvent, repeat above process and can make aqueous solution of chloraurate all be transferred in the organic facies; Under agitation in the toluene that contains gold chloride (or chloroform) solution, dropwise add 0.1M sodium borohydride frozen water solution, become redness, obtain the gold colloidal (probe 2) of the hydrophobization of CTAB protection until xanchromatic toluene solution.
The fingerprint manifestation method: at room temperature, the A4 pattern product that are printed on latent fingerprint earlier soak 2～5min in water after, put into probe 2 and soak 5～15min, take out sample and immerse in the silver-colored dye liquor after with the clear water rinsing, several minutes (as 5min) back is taken out and is dried.
(2) aurosol of Surfactant CTAB modification is a probe 3: under the room temperature, and 5 * 10
-4～10
-3The aqueous solution of M gold chloride and 0.01～0.02M CTAB also stirs; Add 0.01～0.1M sodium borohydride frozen water solution reduction, obtain the nano gold sol (probe 3) of light red CTAB protection.
The fingerprint manifestation method: the latent fingerprint sample is put into probe 3 and is soaked 5～15min after soaking in petroleum ether earlier, takes out to immerse in the silver-colored dye liquor after sample cleans with petroleum ether, and several minutes (as 5min) back is taken out and dried, and promptly obtains the fingerprint that manifests.
Three, the nano gold sol of cysteine functionalization is probe 4 preparation and process for show: under the room temperature, aqueous solution of chloraurate under vigorous stirring by sodium borohydride frozen water solution reduction, then add L-cysteine aqueous solution, continue to stir 10～30min, obtain the gold colloidal of L-cysteine functionalization.
The fingerprint manifestation method: identical with probe 2, just probe 4 replaces probe 2.
The present invention utilizes the nanogold particle of functionalization as the probe recognition objective, in conjunction with the increase signal of nanogold particle identification of argentation, reaches the purpose that manifests clear fingerprint.The nanogold particle of functionalization earlier with latent fingerprint in material effects such as oils, amino acids, then under the condition that the hydroquinone Reducing agent exists, but nanogold particle catalysis Ag
+Be reduced into Ag
0, the silver nano-grain of generation coats around the gold grain, makes the nanogold particle identifying information extended, and latent fingerprint is manifested and can directly be observed by bore hole.Compare the present invention with traditional method and have following advantage:
1, method is simple, quick, selectivity is good; The probe reaction process is simple, easy to operate.
2, not by instrument (bore hole observation) can discern and manifest latent fingerprint; All obtain manifests fingerprint and can directly take pictures under natural light and fetch data.
3, probe is easily preserved; Repeatedly reusable, each operation only needs the silver-colored dye liquor of new preparation to get final product, and during storage, probe 1, probe 2 are preserved some months usually and do not changed under 4 ℃ of conditions, and probe 3, probe 4 are preserved at normal temperatures and got final product.
4, fingerprint image and substrate contrast is clear, and retention time is long.
5, probe is safe in utilization, and the operator is had no side effect.
Novel finger print provided by the invention manifests reagent and process for show thereof, the probe that the nano gold sol of use finishing manifests as latent fingerprint, and highly sensitive, easy to operate, selectivity is good, and the operator is had no side effect, and application prospect is good.
Description of drawings
Accompanying drawing 1, be used for latent fingerprint and manifest the fingerprint image that obtains for probe 1;
Accompanying drawing 2, be used for latent fingerprint and manifest the fingerprint image that obtains for probe 1;
Accompanying drawing 3, be used for latent fingerprint and manifest the fingerprint image that obtains for probe 2;
Accompanying drawing 4, be used for latent fingerprint and manifest the fingerprint image that obtains for probe 2;
Accompanying drawing 5, be used for latent fingerprint and manifest the fingerprint image that obtains for probe 3;
Accompanying drawing 6, be used for latent fingerprint and manifest the fingerprint image that obtains for probe 4.
The specific embodiment
Embodiment 1:
Mercaptan decorated nanometer gold grain is the preparation and the fingerprint manifestation method-particulate preparation of (one) lauryl mercaptan modified nano gold of probe 1:
(1) under the room temperature, the aqueous solution of chloraurate of 30mmol/L mixes with the toluene solution of the four octyl group ammonium bromide of 50mmol/L and stirs, and is transferred to fully in the organic facies toluene up to gold chloride;
(2) in organic facies, add lauryl mercaptan;
(3) follow violent stirring, the sodium borohydride frozen water solution of 0.4mol/L of preparation is newly joined in the mixed solution lentamente, after continuing to stir 3h organic facies is separated;
(4) rotary evaporation surplus solution under 40 ℃ of conditions adds ethanol then and is placed on-18 ℃ of maintenance 4h, and the atropurpureus that obtains precipitation is the gold nano grain of the lauryl mercaptan protection of hydrophobization.
Fingerprint manifestation process: at room temperature, probe 1 (gold nano grain of lauryl mercaptan functionalization) is distributed in the petroleum ether by 0.05% (w/v) concentration, make gold colloidal, make the A4 pattern product that are printed on latent fingerprint behind water logging bubble 2min, put into gold colloidal and soak 5-10min, take out sample clear water rinsing, immerse in the silver-colored dye liquor for preparing then, take out behind about 5min and dry, latent fingerprint manifests also and can directly observe fetch data (accompanying drawing 1) of can directly taking pictures by bore hole under natural light in the sample.
The compound method of silver dye liquor: (1) 10mL citric acid solution pH=3.5; (2) hydroquinone 1g is dissolved in the 30mL water; (3) silver nitrate of 0.2-0.4g (or silver acetate) is dissolved in the 2mL water; (4) the first two is planted and mixes after solution dissolves fully, is facing with preceding adding silver nitrate solution.
Embodiment 2:
Mercaptan decorated nanometer gold grain is the preparation of probe 1 and the preparation and the fingerprint manifestation method of the nanogold particle that fingerprint manifestation method-(two) Stearyl mercaptan is modified: except replace lauryl mercaptan with Stearyl mercaptan, all the other preparation process are identical with the preparation process of the gold nano grain of lauryl mercaptan protection;
Fingerprint manifestation process: identical with the nanogold particle of lauryl mercaptan functionalization (accompanying drawing 2).
Embodiment 3:
The gold colloidal of the hydrophobization that Surfactant CTAB is modified is the preparation and the fingerprint manifestation process of probe 2:
Preparation: under (1) room temperature, 2mM cetyl trimethyl ammonium bromide toluene solution is mixed with 1% aqueous solution of chloraurate, behind the vigorous stirring 5min, static layering is isolated toluene layer to another container; (2) the cetyl trimethyl ammonium bromide toluene solution that adds again in remaining aqueous solution of chloraurate with concentration still can make aqueous solution of chloraurate transfer in the organic solvent toluene, repeats above process and can make aqueous solution of chloraurate all be transferred in the toluene; (3) under agitation in the toluene solution that contains gold chloride, dropwise add 0.1M sodium borohydride frozen water solution, become redness, obtain the gold colloidal (probe 2) of the hydrophobization of CTAB protection until xanchromatic toluene solution.
The fingerprint manifestation process: at room temperature, the A4 pattern product that are printed on latent fingerprint behind the immersion 2min, are put into probe 2 and are soaked 5～15min in water earlier, take out and immerse in the silver-colored dye liquor after sample is used the clear water rinsing, and (accompanying drawing 3) dried in taking-up behind about 5min.
Replace toluene as solvent with chloroform, also can obtain the gold colloidal (probe 2) of the hydrophobization of CTAB protection, fingerprint manifestation process and toluene solvant probe 2 identical (accompanying drawing 4) by above-mentioned experimentation.
Embodiment 4:
The aurosol that Surfactant CTAB is modified is the preparation and the fingerprint manifestation process of probe 3:
Preparation: under (1) room temperature, 5 * 10
-4The aqueous solution of M gold chloride and 0.02M CTAB also stirs; (2) add 0.01M sodium borohydride frozen water solution reduction, obtain the nano gold sol (probe 3) of light red CTAB protection.
The fingerprint manifestation process: the latent fingerprint sample is put into probe 3 and is soaked 5-10min after soaking in petroleum ether earlier, takes out to immerse in the silver-colored dye liquor after sample cleans with petroleum ether, and about 5min takes out and dries, and promptly obtains the fingerprint (accompanying drawing 5) that manifests.
Embodiment 5:
The nano gold sol of cysteine functionalization is the preparation and the fingerprint manifestation method of probe 4:
Preparation: under the room temperature, 10
-4The aqueous solution of chloraurate of M by 0.01g sodium borohydride frozen water solution reduction, then adds 2 * 10 under vigorous stirring
-4M L-cysteine aqueous solution continues to stir 20min, obtains the gold colloidal (probe 4) of L-cysteine functionalization.
The fingerprint manifestation process: the latent fingerprint sample behind water logging bubble 2min, is put into probe 4 and is soaked 5-10min earlier, after the taking-up sample is used the clear water rinsing, immerses in the silver-colored dye liquor for preparing, and takes out behind about 5min and dries, and promptly obtains the fingerprint (accompanying drawing 6) that manifests.
Claims (9)
1, the preparation method of mercaptan modified nano gold particle probe 1, it is characterized in that: under the room temperature, the aqueous solution of chloraurate of 20～50mmol/L mixes with the toluene solution of 40～80mmol/L, four octyl group ammonium bromide and stirs, and phase transfer reagent four octyl group ammonium bromide are transferred to gold chloride in the organic facies toluene fully; In organic facies, add 12 or Stearyl mercaptan then; Follow violent stirring; join the sodium borohydride frozen water solution of 0.1～0.4mol/L of preparation newly in the mixed solution lentamente; after continuing to stir 2～3h organic facies is separated; rotary evaporation surplus solution under 30～50 ℃ of conditions; add ethanol then and be placed on-18～20 ℃ and leave standstill 2～4h, the atropurpureus that obtains precipitation is the gold nano grain probe 1 of the alkyl hydrosulfide protection of hydrophobization.
2, mercaptan as claimed in claim 1 is modified the preparation method of gold nano grain probe 1, it is characterized in that:
(1) under the room temperature, the aqueous solution of chloraurate of 30mmol/L mixes with the toluene solution of the four octyl group ammonium bromide of 50mmol/L and stirs, and is transferred to fully in the organic facies toluene up to gold chloride;
(2) in organic facies, add lauryl mercaptan;
(3) follow violent stirring, the sodium borohydride frozen water solution of 0.4mol/L of preparation is newly joined in the mixed solution lentamente, after continuing to stir 3h organic facies is separated;
(4) rotary evaporation surplus solution under 40 ℃ of conditions adds ethanol then and is placed on-18 ℃ of maintenance 4h, and the atropurpureus that obtains precipitation is the gold nano grain probe 1 of the lauryl mercaptan protection of hydrophobization.
3, mercaptan modification gold nano grain probe 1 as claimed in claim 1 is used for the fingerprint process for show, it is characterized in that: at room temperature, with probe 1 by weight volume ratio 0.01～0.05% concentration be distributed to and make gold colloidal in the petroleum ether, make the A4 pattern product that are printed on latent fingerprint behind water logging bubble 2～5min, put into gold colloidal and soak 5～15min, take out sample clear water rinsing, immerse in the silver-colored dye liquor for preparing then, take out after several minutes and dry, latent fingerprint manifests also and can directly observe by bore hole in the sample;
The compound method of silver dye liquor: (1) 10mL citric acid solution pH=3.5; (2) hydroquinone 1g is dissolved in the 30mL water; (3) silver nitrate of 0.2-0.4g or silver acetate are dissolved in the 2mL water; (4) the first two is planted and mixes after solution dissolves fully, is facing with preceding adding silver nitrate solution.
4, the preparation method of the colloidal gold probe 2 of the hydrophobization of Surfactant CTAB modification, it is characterized in that: under the room temperature, 2mM cetyl trimethyl ammonium bromide toluene or chloroformic solution are mixed with 0.5～5% aqueous solution of chloraurate, behind vigorous stirring 2～5min, static layering is isolated organic layer as in another container; In remaining aqueous solution of chloraurate, add cetyl trimethyl ammonium bromide toluene or chloroformic solution again and still can make aqueous solution of chloraurate continue phase transfer to organic solvent, repeat above process and can make aqueous solution of chloraurate all be transferred in the organic facies; Under agitation in toluene that contains gold chloride or chloroformic solution, dropwise add 0.1M sodium borohydride frozen water solution, become redness, obtain the colloidal gold probe 2 of the hydrophobization of CTAB protection until xanchromatic toluene solution.
5, the colloidal gold probe 2 of the hydrophobization of Surfactant CTAB modification as claimed in claim 4 is used for the fingerprint method for visualizing, it is characterized in that: at room temperature, the A4 pattern product that are printed on latent fingerprint earlier soak 2～5min in water after, put into probe 2 and soak 5～15min, take out and immerse in the silver-colored dye liquor after sample is used the clear water rinsing, the back is taken out and is dried after several minutes.
6, the aurosol of Surfactant CTAB modification is the preparation method of probe 3, it is characterized in that: under the room temperature, and 5 * 10
-4～10
-3The aqueous solution of M gold chloride and 0.01～0.02M CTAB also stirs; Add 0.01～0.1M sodium borohydride frozen water solution reduction, obtain the nano gold sol probe 3 of light red CTAB protection.
7, the aurosol of Surfactant CTAB modification as claimed in claim 6 is that probe 3 is used for the fingerprint method for visualizing, it is characterized in that: after the latent fingerprint sample soaks in petroleum ether earlier, put into probe 4 and soak 5～15min, taking out sample cleans in the silver-colored dye liquor of back immersion with petroleum ether, take out after several minutes and dry, promptly obtain the fingerprint that manifests.
8, nano gold sol probe 4 preparation methoies of cysteine functionalization: it is characterized in that: under the room temperature, aqueous solution of chloraurate under vigorous stirring by sodium borohydride frozen water solution reduction, then add L-cysteine aqueous solution, continue to stir 10～30min, obtain the colloidal gold probe 4 of L-cysteine functionalization.
9, the nano gold sol probe 4 of cysteine functionalization as claimed in claim 7 is used for the fingerprint method for visualizing, it is characterized in that: the nano gold sol probe 4 of usefulness cysteine functionalization replaces the colloidal gold probe 2 of the hydrophobization of Surfactant CTAB modification, and all the other are identical with claim 5.
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