CN101571480B - Surface plasma resonance detection method of morphine - Google Patents
Surface plasma resonance detection method of morphine Download PDFInfo
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- CN101571480B CN101571480B CN2009100859349A CN200910085934A CN101571480B CN 101571480 B CN101571480 B CN 101571480B CN 2009100859349 A CN2009100859349 A CN 2009100859349A CN 200910085934 A CN200910085934 A CN 200910085934A CN 101571480 B CN101571480 B CN 101571480B
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Abstract
The invention discloses a surface plasma resonance detection method of morphine, belonging to the detection technical field. A morphine molecular identification sensitive chip of an optical sensor is taken as a sensing chip of a surface plasma resonance detector, and the surface plasma resonance detector is utilized to detect light intensity change of total reflected light at the interface betweena sample to be detected and the molecular identification sensitive chip to directly determine the morphine content in the sample to be detected when the sample to be detected passing through the sens ing chip surface. The detection method has the characteristics of severe environment resistant, high selectivity, fast response and simple operation and not only improves the sensitivity of the methodbut also reduces detection cost accordingly.
Description
Technical field
The invention belongs to the detection technique field, relate to a kind of surface plasma resonance rapid detection method of morphine.
Background technology
(Morphine is a kind of morphinane alkaloid that extracts from opium MO) to morphine, is the effective constituent main in the opium, that content is maximum, and average content is 10%.Morphine is widely used in clinical treatment because of it has strong analgesic activity.But the very easily habituation of morphine makes long-term smoker still all can produce severe dependency to morphine psychologically from health, causes serious toxicomania.Morphine is mixed various chemical medicaments again, through further processing, promptly becomes the bigger heroin of toxicity.The abuse of morphine drugs has brought great harm for people's life and lives and properties.Therefore, no matter in forensic science work or in the medical monitoring process, realize to morphine and metabolin thereof trace, sensitivity, accurately, the detection changed fast and automatically is extremely important.
At present, the drug test field is more at the detection method of morphine, has almost related to all technology of modern analysis chemistry.For many years, because chromatography has the separation efficiency height, analysis speed is fast, selectivity good and polycomponent such as analyzes simultaneously at advantage, particularly the conventional sense task of people to the medicine morphine born in it and mass spectroscopy coupling (GC/MS) always.Yet, it needs instrument and equipment, the those skilled in the art of complicated sample pre-treatment process, costliness, finish in addition and once analyze time-consuming and expense is high, be difficult to satisfy the quick and on-the-spot needs that detect of a large amount of samples in the present drug surveillance, this just requires more novel Fast Detection Technique to occur.
(Surface Plasmon Resonance SPR) is a kind of physical optics phenomenon, and it studies the chemistry and the physisorption character of material by the variation of measuring the metal surface material refractive index in surface plasma wave resonance.Sensor and applied research thereof based on the SPR principle obtained significant progress in recent ten years.Compare with the conventional sense technology, it has high sensitivity, response is fast, volume is little, physical strength is big, testing process is quick, can obtain real time data, easy to operate, need not mark, the biologically active that can keep molecule, anti-electromagnetic interference capability is strong with the optical fiber outstanding advantages such as the remote collection that can realize data and continuous on-line monitoring that link to each other.At present, the research that the SPR sensing technology is used for the morphine detection both at home and abroad reports that also seldom only several pieces of reports mainly are based on traditional SPR immune sensing technology, by the detection of competition law realization to the morphine molecule.For example, Ri Ben people such as Go Sakai have studied success and utilize surface plasma resonance biosensor to pass through the detection of solution competition law to Morphine in Urine.
The research of immunoassay aspect be the SPR sensing technology use the time the earliest, one of range of application is the widest, development is the most perfect field, yet since technology have need zoopery, to testing environment requirement harshness, involve great expense and the chip repeat performance shortcoming that is difficult to overcome such as relatively poor, therefore limited the SPR sensing technology in morphine detects development.
On the basis of the drug morphia molecular recognition sensitivity chip of a kind of optical sensor that we report in number of patent application is 200910119164.5 patent of invention, mating surface plasma resonance detector provides a kind of method for surface plasmon resonance detection of morphine.
Summary of the invention
Problems such as the objective of the invention is when detecting morphine, to exist testing environment requirement harshness, involve great expense, selectivity is relatively poor in order to solve existing SPR technology, a kind of surface plasma resonance rapid detection method of morphine is provided, can be applied to the direct detection of batch samples morphine in the organic solvent.
The objective of the invention is to be achieved through the following technical solutions.
The present invention is with a kind of drug morphia molecular recognition sensitivity chip of the optical sensor sensing chip as the surface plasma body resonant vibration detector, when testing sample by sensing chip when surface, utilize the surface plasma body resonant vibration detector detect testing sample and molecular recognition sensitive chip at the interface the light intensity variation of total reflection light directly measure morphine content in the testing sample.The concrete operations step is as follows:
(1) drug morphia molecular recognition sensitivity chip with optical sensor is fixed in the surface plasma body resonant vibration detector as sensing chip;
(2) organic solvent is flow through the sense chip surface, treat that reflective light intensity reaches to stablize when constant, reflective light intensity is scanned by angle, note the SPR spectrogram;
(3) get the morphine standard solution of variable concentrations,, flow through the surface of surface plasma resonance sensing chip respectively according to by the order of low concentration to high concentration;
The certain density morphine titer of each inflow, with sensing chip reaction 1～5min, flow through organic solvent then, treat that reflective light intensity reaches and stablize when constant, reflective light intensity is scanned by angle, note the morphine titer of this concentration and the SPR spectrogram after the sensing chip generation adsorption reaction, so far finish the detection of the morphine titer of a concentration;
The rest may be inferred, up to morphine standard solution that obtains each concentration and the reacted SPR spectrogram of sensing chip.
(4) respectively the morphine standard solution of the variable concentrations that obtains in (3) and the reacted SPR spectrogram of sensing chip and SPR spectrogram in (2) are compared, calculate the shift value Δ θ of the SPR resonance angle that causes before and after the adsorption reaction under each concentration;
(5) the shift value Δ θ with the SPR resonance angle is an ordinate, with the negative logarithm of the morphine concentration of standard solution value that adds as horizontal ordinate drawing standard curve;
(6) method of testing of pressing typical curve detects testing sample, causes the shift value Δ θ of SPR resonance angle according to itself and sensing chip generation adsorption reaction front and back, reads the content of morphine on typical curve;
Wherein, the compound method of morphine standard solution is as follows: take by weighing a certain amount of pure morphine solid, add the organic solvent constant volume, the concentration of preparing serial morphine standard solution is 1ppb, 10ppb, 100ppb, 1ppm, 10ppm and 100ppm;
The surface plasma resonance rapid detection method of described a kind of morphine, its described organic solvent is following one or both compound: methylene chloride, methenyl choloride, methyl alcohol, acetonitrile, N, dinethylformamide, sulfone compound or heterocycle compound;
Beneficial effect of the present invention is:
This law invention utilizes the sensing chip of a kind of drug morphia molecular recognition sensitivity chip of optical sensor as the surface plasma body resonant vibration detector,, adopt the content of morphine in the direct SPR detection method working sample.This detection method has response fast, can go out the result in general 5～10min; The selectivity height can effectively be discerned the morphine content in morphine, codeine (monoacetylmorphine) and heroin (biacetyl morphine) biased sample; Easy and simple to handle, the direct morphine content in the working sample has been avoided the loaded down with trivial details step of indirect detection method; Anti-adverse environment, for immunologic method, this method can realize the detection to morphine in high temperature, high pressure, acid, alkali and organic solvent, is difficult for being destroyed by biodegradation; Not only improve the sensitivity of method, also correspondingly reduced the detection cost.
Description of drawings
Fig. 1 is a canonical plotting in the embodiment of the invention
Specific embodiment
The present invention is a kind of method for surface plasmon resonance detection of morphine.It is to utilize the SPR detector that has surface plasma resonance sensor, be penetrated into the evanescent wave that produces in the metallic film by incident light at the interface during experiences total internal reflection at optical cover slide and metallic film, the free electron that causes the metallic film surface produces surface plasma, in incident angle is under the condition of a certain appropriate value, and surface plasma and evanescent wave resonate.We are with a kind of drug morphia molecular recognition sensitivity chip of the optical sensor sensing chip as the surface plasma body resonant vibration detector, when testing sample is surperficial by sensing chip, if wherein contain the surface that the morphine molecule will be adsorbed to sensing chip, cause the refractive index of metallic film near surface to change, thereby cause catoptrical light intensity to change, detect the just direct content of morphine in the working sample of this variation.
The present invention is with a kind of drug morphia molecular recognition sensitivity chip of the optical sensor sensing chip as the surface plasma body resonant vibration detector, and when testing sample during by the sensing chip surface, the SPR detector is the morphine content in the working sample directly; The concrete operations step is as follows:
(1) at first on the optical cover slide, plate the thick golden film of one deck 47nm by vacuum vapor deposition method, with this as golden film substrate.The microsphere morphine of 0.0077g (0.025mmol) is joined bottom in the 5ml round-bottomed flask, and be placed in 115 ℃ the oil bath and heat 15min, then to wherein adding methacrylic acid 0.0086g (0.1mmol), after treating the two formation oily mater, add the crosslinking chemical ethylene glycol dimethacrylate of 0.0496g (0.25mmol), the acetonitrile of 1.0ml and the initiating agent azoisobutyronitrile of 0.0030g more successively, behind the ultrasonication 5min, logical nitrogen deoxygenation 10mim; Peek is dripped drips of solution and is added on the silanization microslide that is stained with support membrane, covers golden film substrate, and with clip the two is clamped; With above-mentioned make bilayer reaction sheet put into closed reactor, under nitrogen protection, in 65 ℃ of water-baths, added thermal response 5 hours; Reaction after finishing separates microslide and golden film substrate, can be inlaid with the functional polymer polymer film of morphine molecule at the crosslinked last layer of golden film substrate surface; Utilizing volume ratio is that the mixed liquor of 9: 1 acetonitrile and acetate is removed the morphine molecule in the functional polymer polymer film.After wash-out finishes, the gained chip is dried to weight under vacuum condition, obtains being used for the drug morphia molecular recognition sensitivity chip of optical sensor at last.
(2) drug morphia molecular recognition sensitivity chip with optical sensor is fixed in the surface plasma body resonant vibration detector as sensing chip;
(3) acetonitrile is flow through the sense chip surface, treat that reflective light intensity reaches to stablize when constant, reflective light intensity is scanned by angle, note the SPR spectrogram;
(4) get the morphine standard solution of variable concentrations,, flow through the surface of surface plasma resonance sensing chip respectively according to by the order of low concentration to high concentration;
The certain density morphine titer of each inflow, with sensing chip reaction 5min, flow through acetonitrile then, treat that reflective light intensity reaches and stablize when constant, reflective light intensity is scanned by angle, note the morphine titer of this concentration and the SPR spectrogram after the sensing chip generation adsorption reaction, so far finish the detection of the morphine titer of a concentration; The rest may be inferred, up to morphine standard solution that obtains each concentration and the reacted SPR spectrogram of sensing chip.
(5) respectively the morphine standard solution of the variable concentrations that obtains in (4) and the reacted SPR spectrogram of sensing chip and SPR spectrogram in (3) are compared, calculate the shift value Δ θ of the SPR resonance angle that causes before and after the adsorption reaction under each concentration;
(6) the shift value Δ θ with the SPR resonance angle is an ordinate, with the negative logarithm of the morphine concentration of standard solution value that adds as horizontal ordinate drawing standard curve, as shown in Figure 1.
(7) method of testing of pressing typical curve detects testing sample, causes the shift value Δ θ of SPR resonance angle according to itself and sensing chip generation adsorption reaction front and back, reads the content of morphine on typical curve;
Wherein, the compound method of morphine standard solution is as follows: take by weighing a certain amount of pure morphine solid, add the acetonitrile constant volume, the concentration of preparing serial morphine standard solution is 1ppb, 10ppb, 100ppb, 1ppm, 10ppm and 100ppm;
Claims (2)
1. the method for surface plasmon resonance detection of a morphine utilizes surface plasma body resonant vibration SPR detector, and detection testing sample and molecular recognition the sensitive chip light intensity of total reflection light at the interface change the morphine content of directly measuring in the testing sample; It is characterized in that: with a kind of drug morphia molecular recognition sensitivity chip of the optical sensor sensing chip as the surface plasma body resonant vibration detector, when testing sample during by the sensing chip surface, the SPR detector is the morphine content in the working sample directly; The concrete operations step is as follows:
(1) drug morphia molecular recognition sensitivity chip with optical sensor is fixed in the surface plasma body resonant vibration detector as sensing chip;
(2) organic solvent is flow through the sensing chip surface, treat that reflective light intensity reaches to stablize when constant, reflective light intensity is scanned by angle, note the SPR spectrogram;
(3) get the morphine standard solution of variable concentrations,, flow through the surface of surface plasma resonance sensing chip respectively according to by the order of low concentration to high concentration;
The certain density morphine titer of each inflow, with sensing chip reaction 1～5min, flow through organic solvent then, reflective light intensity is scanned by angle, note the morphine titer of this concentration and the SPR spectrogram after the sensing chip generation adsorption reaction, so far finish the detection of the morphine titer of a concentration;
The rest may be inferred, up to morphine standard solution that obtains each concentration and the reacted SPR spectrogram of sensing chip;
(4) respectively the morphine standard solution of the variable concentrations that obtains in (3) and the reacted SPR spectrogram of sensing chip and SPR spectrogram in (2) are compared, calculate the shift value Δ θ of the SPR resonance angle that causes before and after the adsorption reaction under each concentration;
(5) the shift value Δ θ with the SPR resonance angle is an ordinate, with the negative logarithm of the morphine concentration of standard solution value that adds as horizontal ordinate drawing standard curve;
(6) method of testing of pressing typical curve detects testing sample, causes the shift value Δ θ of SPR resonance angle according to itself and sensing chip generation adsorption reaction front and back, reads the content of morphine on typical curve;
Wherein, the compound method of morphine standard solution is as follows: take by weighing a certain amount of pure morphine solid, add the organic solvent constant volume, the concentration of preparing serial morphine standard solution is 1ppb, 10ppb, 100ppb, 1ppm, 10ppm and 100ppm; Following one or both the compound of described organic solvent: methylene chloride, methenyl choloride, toluene, methyl alcohol, acetonitrile, N, dinethylformamide, sulfone compound or heterocycle compound.
2. the method for surface plasmon resonance detection of a kind of morphine according to claim 1, its described drug morphia molecular recognition sensitivity chip method for making is at first to plate the thick golden film of one deck 47nm by vacuum vapor deposition method on the optical cover slide, with this as golden film substrate; The microsphere morphine of 0.0077g is joined bottom in the 5ml round-bottomed flask, and be placed in 115 ℃ the oil bath and heat 15min, then to wherein adding methacrylic acid 0.0086g, after treating the two formation oily mater, add the crosslinking chemical ethylene glycol dimethacrylate of 0.0496g, the acetonitrile of 1.0ml and the initiating agent azoisobutyronitrile of 0.0030g more successively, behind the ultrasonication 5min, logical nitrogen deoxygenation 10min; Peek is dripped drips of solution and is added on the silanization microslide that is stained with support membrane, covers golden film substrate, and with clip the two is clamped; The bilayer reaction sheet of making is put into closed reactor, under nitrogen protection, in 65 ℃ of water-baths, added thermal response 5 hours; Reaction after finishing separates microslide and golden film substrate, can be inlaid with the functional polymer polymer film of morphine molecule at the crosslinked last layer of golden film substrate surface; Utilizing volume ratio is that the mixed liquor of 9: 1 acetonitrile and acetate is removed the morphine molecule in the functional polymer polymer film; After wash-out finishes, the gained chip is dried to weight under vacuum condition, obtains being used for the drug morphia molecular recognition sensitivity chip of optical sensor at last.
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| CN103234940B (en) * | 2013-05-14 | 2015-05-13 | 北京理工大学 | Molecular imprinting sensing chip available for underwater detection |
| CN103884673B (en) * | 2014-03-31 | 2017-04-26 | 西安交通大学 | Online infrared spectroscopy monitoring system and method for hard drug taking condition |
| CN105300931A (en) * | 2015-10-14 | 2016-02-03 | 温州生物材料与工程研究所 | Portable surface plasma resonance biochemical detection device based on intelligent mobile phone as well as portable mobile phone accessories and application thereof |
| CN106896086A (en) * | 2016-10-08 | 2017-06-27 | 浙江警察学院 | A kind of morphine detection method based on SPR technique |
| CN107345909A (en) * | 2017-06-23 | 2017-11-14 | 浙江诺迦生物科技有限公司 | The detection method of trace morphine and the SPR chips used in a kind of saliva sample |
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