CN112578017B - Rapid detection method and detection device for organic matters in high-salinity water - Google Patents
Rapid detection method and detection device for organic matters in high-salinity water Download PDFInfo
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- CN112578017B CN112578017B CN202011256462.1A CN202011256462A CN112578017B CN 112578017 B CN112578017 B CN 112578017B CN 202011256462 A CN202011256462 A CN 202011256462A CN 112578017 B CN112578017 B CN 112578017B
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Abstract
The invention discloses a method and a device for rapidly detecting organic matters in high-salinity water, and relates to the technical field of detection of organic pollutants in water. The invention is based on the self-evaporation desalination means and the substance similarity intermiscibility principle, and realizes the rapid separation of inorganic salt and organic matter in high-salinity water; the electrospray ionization mass spectrometry is adopted to detect the organic matter type in the high-salinity water, and in the testing process, the performance indexes such as precision, accuracy, sensitivity and the like in the detection application process of the device are comprehensively evaluated, so that the technical problem that the organic pollutants are difficult to rapidly and accurately detect in the high-salinity environment is finally solved, an effective technical means is provided for qualitative and quantitative analysis of the organic pollutants, and powerful scientific and technological support is provided for ecological environment protection, food safety detection and the like. The detection equipment applied in the detection method is provided with the mass spectrum detector, the three-dimensional adjusting carrying platform and the heating device, and the equipment is simple, light, low in cost and easy to popularize and apply.
Description
Technical Field
The invention relates to the technical field of detection of organic pollutants in water, in particular to a rapid detection method and a rapid detection device for organic matters in high-salinity water.
Background
Most of the existing methods for detecting organic pollutants in seawater are complex sample pretreatment processes such as auxiliary solid phase extraction, novel needle catcher, stirring rod adsorbent extraction and the like, which not only consumes time and has high cost, but also can cause secondary loss or pollution of samples due to complex operation steps, and are difficult to be widely applied.
In recent years, atmospheric pressure ionization mass spectrometry has shown excellent performance in rapidly analyzing complex samples. This type of method requires only a simple sample pretreatment step, and even in some cases no sample pretreatment. During measurement, a sample to be detected can be directly desorbed and ionized on a matrix and then enters a mass spectrum for analysis, and the method has great potential in the aspect of detection of some high-salt samples. Furthermore, nanoelectrospray coupled with ionic electromigration provides satisfactory mass spectral data in the presence of physiological or higher concentrations of salt (e.g., 150mmol/L aqueous NaCl, 150mmol/L KCl and 25mmol/L Tris-HCl buffer, urine, and tears). However, these techniques have not been practical for real seawater samples with salinity higher than 599mmol/L, and due to ionic electromigration, salt ions will desorb/ionize before the target analyte, contaminating the mass spectrometer detector, reducing the signal of the target. Therefore, there is a need to develop a new analysis technique for realizing rapid and direct detection of organic pollutants in seawater.
Disclosure of Invention
The invention provides a rapid detection method and a detection device for organic matters in high-salinity water, aiming at the technical problems in the prior detection technology.
The invention is based on the self-evaporation desalination means and the substance similarity intermiscibility principle, and realizes the rapid separation of inorganic salt and organic matter in high-salinity water; and (3) accurately detecting the organic matter type in the high-salinity water by adopting an electrospray ionization mass spectrometry, and comprehensively evaluating performance indexes such as precision, accuracy, sensitivity, detection limit and the like in the detection application process of the device in the test process.
In order to solve the technical problem, the equipment applied in the detection method is provided with a mass spectrometer, a three-dimensional adjusting loading platform and a heating device, and the detection method comprises the following steps:
1) placing a metal sheet with a tip on a heating device, wherein the heating device is arranged on a three-dimensional adjusting carrying platform, and adjusting the three-dimensional adjusting carrying platform to enable the tip of the metal sheet to be over against the center of a mass spectrum sample inlet of a mass spectrum detector;
2) dripping a sample to be detected to the tip position of the metal sheet, wherein the dripped sample to be detected is usually 5 mu L, the tip is a sample carrying angle, then, a heating switch of a heating device is turned on, the metal sheet starts to heat up, the water in the sample solution starts to evaporate, inorganic salt crystals and organic matters are separated out and are left at the tip of the metal sheet;
3) after all solvents are completely evaporated, closing the heating device, dropwise adding an organic solvent to the tip of the metal sheet with the crystallization salt and the organic matters, according to the principle of matter similarity and intermiscibility, quickly dissolving the organic matters separated out before in the organic solvent to form an organic solution, and keeping the salt on the metal sheet in a crystal state;
4) and 3.5-5.0 kilovolt voltage is introduced through the conductive electrode which is contacted with the rear end of the metal sheet, and at the moment, a high-voltage electric field is formed between the tip of the metal sheet and the mass spectrum sample inlet, so that the solution containing the organic matters is sprayed out from the tip of the metal sheet, electrospray ionization is generated, and the solution enters a mass spectrum detector for sample analysis, and the detection of the organic matters in the high-salt sample solution is completed.
Preferably, the size of the metal sheet is 20mm multiplied by 0.15mm, and the material of the metal sheet is corrosion-resistant metal material.
Preferably, the distance between the tip of the metal sheet and the center of the mass spectrum injection port is 2mm-5 mm.
Preferably, the amount of the sample to be tested dropped in the step 2) is 5. mu.L.
Preferably, the heating device is an electric heating wire heating device, and the heating temperature of the electric heating wire heating device in the step 2) is controlled to be between 40 ℃ and 80 ℃.
Preferably, the organic solvent added dropwise in step 3) is methanol or acetonitrile.
Compared with the prior art, the invention has the following beneficial effects:
1) the invention utilizes the principles of self-evaporation desalination and substance similarity intermiscibility to realize the rapid separation of inorganic salt and organic analytes in seawater samples, does not need complex sample pretreatment, simplifies the operation steps, avoids the secondary pollution and loss of the samples, has short time consumption and realizes the rapid and sensitive detection of organic pollutants in the seawater.
2) The invention is based on the electrospray ion source mass spectrum technology, not only avoids the pollution of salt (sodium chloride and the like) to the mass spectrum, but also reduces the sample introduction amount and the reagent consumption, and has high accuracy and low cost.
3) The three-dimensional adjusting loading platform and the heating wire heating module have the advantages of simple structure and small volume, and the metal sheet which is corrosion-resistant, fast in heat conduction and fast in electric conduction is used as a sample carrier, so that the sample crystallization time can be greatly shortened; the combination mass spectrum is used for analysis, so that the data is more visual and accurate, and the reliability of the detection data is improved.
Drawings
FIG. 1 is a schematic structural view of a three-dimensional adjustable loading platform carrying a metal sheet and a heating module according to the present invention;
FIG. 2 is a schematic diagram of the self-desalination mechanism of the present invention;
FIG. 2a is a schematic view of a crystal formed on a metal sheet before detection;
FIG. 2b is a schematic view of a partially enlarged image of FIG. 2 a;
FIG. 2c is a schematic crystal diagram of the surface of the metal sheet after the detection;
FIG. 2d is a schematic view of the enlarged partial image of FIG. 2 c;
FIG. 3 is a schematic mass spectrum of the antibiotic rifampicin RFP of the present invention.
The symbols in the figures indicate:
1. a heating wire heating device; 2. a metal sheet; 3. a high voltage input electrode; 4. and a mass spectrum sample inlet.
Detailed Description
The invention is further described below in conjunction with the drawings and the specific embodiments to assist in understanding the contents of the invention. Terms used in the present invention are all terms that are conventional in the industry, unless otherwise specified.
The invention provides a method for rapidly detecting organic matters in high-salinity water, which is based on the principle of self-evaporation desalination and substance similarity and intermiscibility and an electrospray ionization mass spectrometry technology and is used for rapidly and directly detecting organic pollutants in high-salinity water such as seawater. The detection method comprises the following steps:
1) the metal sheet with the tip end is placed on a heating wire heating device of the detection equipment, the heating wire heating device is arranged on a three-dimensional adjusting carrying platform, the tip end of the metal sheet is enabled to be over against the center of a mass spectrum sample inlet of the mass spectrum detector by adjusting the three-dimensional adjusting carrying platform, and the distance between the tip end of the metal sheet and the center of the mass spectrum sample inlet is 2mm-5 mm.
2) Dropping a sample to be detected to the tip position of the metal sheet, wherein the tip is a sample carrying angle, then opening a heating switch of an electric heating wire heating device, heating the metal sheet through the heating device, controlling the heating temperature to be within the range of 40-80 ℃, starting temperature rise of the metal sheet, starting evaporation of water in a sample solution, and because salt and organic matters have higher boiling points, the salt and the organic matters cannot evaporate along with the evaporation of water, so that inorganic salt is crystallized and separated out and is left at the tip of the metal sheet.
3) After all the solvents are completely evaporated, crystallizing and separating out inorganic salt, closing the electric heating wire heating device, dropwise adding organic solvents such as methanol or acetonitrile and the like to the tip of the metal sheet with the crystallized salt and the organic matters, according to the principle of matter similarity and intermiscibility, the organic matters separated out before can be quickly dissolved in the organic solvents to form organic solutions, and the salts are still left on the metal sheet in a crystal state.
4) At the moment, a voltage of 3.5-5.0 kilovolts is applied to the conductive electrode contacted with the rear end of the metal sheet, a high-voltage electric field is formed between the tip of the metal sheet and the mass spectrum sample inlet, so that the solution containing organic matters is sprayed out from the tip of the metal sheet, electrospray ionization is generated, the solution enters a mass spectrum detector for sample analysis, and the detection of the organic matters in the high-salt sample solution is completed.
As shown in fig. 1, the invention further provides a device for detecting organic matters in high-salt water, the device is a combined device of a three-dimensional adjusting loading platform and a mass spectrum detector, a heating wire heating device is arranged above the three-dimensional adjusting loading platform, and a metal sheet is arranged above the heating wire heating device; three-dimensional regulation cargo platform can carry out around the sheetmetal 10mm, control 10mm and the positive and negative 5 regulation of level, adjusts distance and the angle between sheetmetal spraying tip and the mass spectrum detector mass spectrum introduction port to obtain stronger sample mass spectrum signal, then fixed the front end to the mass spectrum introduction port by a skeleton with whole set of structure again, carry out the linkage operation with the mass spectrum detector, detection equipment is simple, light, with low costs, easily popularization and application.
As a preferred embodiment of the present invention, the length, width and height of the metal sheet in this embodiment are 20mm × 20mm × 0.15mm, and the metal sheet is made of a corrosion-resistant metal material such as stainless steel or platinum sheet.
1. Feasibility test of detection method
In order to verify the reliability and feasibility of the detection result of the method in practical application, the crystallization phenomena of the salt and the target organic substance Rifampicin (RFP) after self-evaporation and detection are observed by a microscope, and the specific tests are as follows:
the process of target analyte generation of ions includes three steps:
(1) separating from the salt by crystallization;
(2) dissolving in a spray solvent;
(3) desorption/ionization.
As shown in fig. 2, fig. 2a and 2b are image evidences of sample separation obtained with a microscope.
The RFP crystallizes on the surface of the cover slip and salt crystals rather than embedding in the salt crystals. The separated crystals of RFP can then be rapidly dissolved using a spray solvent. Finally, a high voltage is applied to the solvent containing the RFP, which forms an electrospray on one corner of the metal plate and enters the mass spectrometer for analysis.
After completion of the detection, the crystal region on the metal sheet was observed again as shown in fig. 2c and 2 d. It is evident from the figure that the target analyte RFP was completely removed and the salt crystals were not damaged, indicating that the RFP sent to mass spectrometry was not contaminated with salts. This confirms the effectiveness of the desalination technique of the present invention.
The invention is based on the aims of serving marine economy and guaranteeing food safety, autonomously develops a rapid detection method for organic pollutants in high-salinity water such as seawater and develops a corresponding detection device, and the technology is based on a self-evaporation desalting means and a substance similarity and intermiscibility principle, so that the rapid separation of inorganic salt and organic matters in the seawater is realized; and (3) accurately detecting the organic matter type in the seawater by adopting an electrospray ionization mass spectrometry. In the testing process, performance indexes such as precision, accuracy, sensitivity, detection limit and the like in the detection application process of the equipment are comprehensively evaluated. Finally, the technical problem that organic pollutants are difficult to detect quickly and accurately in a high-salt environment is solved, an effective technical means is provided for qualitative and quantitative analysis of the organic pollutants, and powerful scientific and technological support is provided for ecological environment protection, food safety detection and the like.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
However, the above description is only exemplary of the present invention, and the scope of the present invention should not be limited thereby, and the replacement of the equivalent components or the equivalent changes and modifications made according to the protection scope of the present invention should be covered by the claims of the present invention.
Claims (6)
1. A rapid detection method for organic matters in high-salinity water is characterized in that the detection method comprises the following steps:
1) placing a metal sheet with a tip on a heating device, wherein the heating device is arranged on the three-dimensional adjusting carrying platform, and adjusting the three-dimensional adjusting carrying platform to enable the tip of the metal sheet to be over against the center of a mass spectrum sample inlet of a mass spectrum detector;
2) dripping a sample to be detected to the tip position of the metal sheet, wherein the tip is a sample carrying angle, then opening a heating switch of the heating device, starting heating the metal sheet, starting evaporation of water in a sample solution, precipitation of inorganic salt crystals and organic matters, and remaining at the tip of the metal sheet;
3) after all solvents are completely evaporated, closing the heating device, dropwise adding an organic solvent to the tip of the metal sheet with the crystallization salt and the organic matters, according to the principle of matter similarity and intermiscibility, quickly dissolving the organic matters separated out before in the organic solvent to form an organic solution, and keeping the salt on the metal sheet in a crystal state;
4) and 3.5-5.0 kilovolt voltage is introduced through the conductive electrode which is contacted with the rear end of the metal sheet, and at the moment, a high-voltage electric field is formed between the tip of the metal sheet and the mass spectrum sample inlet, so that the solution containing the organic matters is sprayed out from the tip of the metal sheet, electrospray ionization is generated, and the solution enters a mass spectrum detector for sample analysis, and the detection of the organic matters in the high-salt sample solution is completed.
2. The method as claimed in claim 1, wherein the size of the metal sheet is 20mm x 0.15mm, and the metal sheet is made of corrosion-resistant metal material.
3. The method for rapidly detecting the organic matters in the high-salinity water according to claim 2, wherein the distance between the tip of the metal sheet and the center of the mass spectrum sample inlet is 2mm-5 mm.
4. The method for rapidly detecting the organic matters in the high-salinity water according to claim 1, wherein the amount of the sample to be detected dripped in the step 2) is 5 μ L.
5. The method for rapidly detecting the organic matters in the high-salinity water according to claim 4, wherein the heating device is a heating wire heating device, and the heating temperature of the heating wire heating device in the step 2) is controlled to be between 40 ℃ and 80 ℃.
6. The method for rapidly detecting the organic matters in the high-salinity water according to claim 1, wherein the organic solvent added dropwise in the step 3) is methanol or acetonitrile.
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