CN114460213B - Real-time online analysis system and method for complex sample - Google Patents
Real-time online analysis system and method for complex sample Download PDFInfo
- Publication number
- CN114460213B CN114460213B CN202011260649.9A CN202011260649A CN114460213B CN 114460213 B CN114460213 B CN 114460213B CN 202011260649 A CN202011260649 A CN 202011260649A CN 114460213 B CN114460213 B CN 114460213B
- Authority
- CN
- China
- Prior art keywords
- sample
- unit
- porous medium
- temperature control
- real
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7233—Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
- G01N30/724—Nebulising, aerosol formation or ionisation
- G01N30/7266—Nebulising, aerosol formation or ionisation by electric field, e.g. electrospray
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to a real-time online analysis system and method for complex samples, belongs to the technical field of organic analytical chemistry, and solves the problems of complex pretreatment, severe dependence on cost chromatograph, frequent cleaning and replacement of chromatographic columns during chromatographic analysis and low separation and detection efficiency in the prior art. The invention discloses a real-time online analysis system for complex samples, which comprises a load unit, a temperature control unit, an ionization unit and a detection unit; the loading unit is a disposable porous medium and is used for loading a sample; the temperature control unit is used for controlling the temperature of the sample loaded on the load unit; an ionization unit for ionizing the sample volatilized from the disposable porous medium; the detection unit is a mass spectrometer for qualitative and quantitative detection of the sample ionized from the ionization unit. The method realizes the direct real-time online analysis and detection of complex samples without treatment and dilution.
Description
Technical Field
The invention relates to the technical field of organic analytical chemistry, in particular to a real-time online analysis system and method for complex samples.
Background
Mass spectrometry has been widely used in the field of mixture analysis and identification due to its rapid analysis speed, high accuracy, good sensitivity, and simultaneous analysis of multiple substances. For more complex actual samples, such as human body fluids used in analyzing the relationship between diseases and metabolites, river water directly collected in analyzing the pollution of river water, petroleum collected for analyzing the components thereof, many complex pretreatment is required, and separation and identification are performed by using a chromatography-mass spectrometry technique. Depending on the actual condition of the sample, these pretreatment operations generally include filtration, dilution, centrifugation, extraction, degradation, etc., which are time-consuming and labor-consuming, and are prone to introduce errors, resulting in a measurement that differs significantly from the actual one. For chromatography-mass spectrometry, a detection laboratory or a detection mechanism is required to be provided with a proper chromatograph, and high performance liquid chromatography or gas chromatography, i.e. gas chromatography or liquid chromatography, is selected according to the situation. Chromatograph cost is not enough, and for many laboratories with common conditions, it is difficult to have two mass spectrometers, and to use them separately in gas chromatography and high performance liquid chromatography. The gas chromatography has high resolution and good separation effect, but the sample to be detected needs to be heated to be completely gasified at high temperature, and liquid chromatography is needed for the sample with high boiling point and difficult gasification. For high performance liquid chromatography, every sample analyzed, one or more washes of the column are required to avoid affecting the subsequent sample determination. In addition, for different samples, it is also necessary to select and replace the appropriate chromatographic column. The pretreatment of the sample and the washing of the chromatographic column greatly affect the detection efficiency of complex actual samples.
Therefore, the prior pretreatment process is complicated in the process of analyzing complex samples, gas chromatography and liquid chromatography which are seriously dependent on the cost are combined with mass spectrometry to form gas chromatography-mass spectrometry equipment and liquid chromatography-mass spectrometry equipment, and meanwhile, the complex chromatographic column is required to be cleaned and replaced, so that the separation and detection efficiency is low.
Disclosure of Invention
In view of the above analysis, the present invention aims to provide a complex sample online analysis system and a use method thereof, which at least solve one of the following technical problems: (1) complex pre-analysis processing; (2) severely relying on inexpensive chromatographs; (3) chromatographic analysis frequently cleans and replaces chromatographic columns; (4) separation and detection efficiency is low.
In one aspect, the invention provides a real-time online analysis system for complex samples, which comprises a load unit, a temperature control unit, an ionization unit and a detection unit;
the loading unit is a disposable porous medium and is used for loading a sample;
the temperature control unit is used for controlling the temperature of the sample loaded on the load unit;
the ionization unit is used for ionizing the sample which is volatilized out of the disposable porous medium;
the detection unit is a mass spectrum.
Further, the disposable porous medium is a glass sand chip and is horizontally placed on the upper surface of the temperature control unit.
Further, the disposable porous medium is cylindrical.
Further, the ionization unit is placed above the load unit, and the tail end of the ionization unit is 2-5mm away from the central axis of the mass spectrum sample inlet.
Further, the ionization unit is a plasma discharge ion source.
Further, the plasma discharge ion source is a glow discharge ion source.
Further, the included angle between the plasma discharge ion source and the horizontal plane is 40-50 degrees.
On the other hand, the invention provides a real-time online analysis method for complex samples, which uses the real-time online analysis system for complex samples and comprises the following steps:
and 5, opening a sample inlet of the detection unit, and enabling all components in the sample to escape and volatilize from the load unit, and enabling the components to enter the detection unit for detection after being ionized by the ionization unit.
Further, in the step 4, the temperature rising rate of the temperature control unit is 1.0-100.0 ℃/min.
Further, in the step 5, qualitative analysis is performed by mass spectrogram of the sample, and quantitative analysis is performed on the sample by drawing an extracted ion flow chromatogram.
Compared with the prior art, the invention has at least one of the following beneficial effects:
(1) The present invention uses a disposable porous medium (e.g., a glass sand chip) to carry the sample. The method directly performs discarding and recycling treatment after each measurement, avoids the repeated use of the gas spectrum column and the liquid spectrum column in the prior art, and effectively avoids the interference between samples. And the chromatographic column does not need to be selectively replaced and cleaned before each sample is analyzed like the existing chromatographic-mass spectrometry technology, so that the separation procedure is greatly saved, and the analysis efficiency is improved.
(2) Compared with the prior art, the method has the advantages that complicated liquid-solid separation operations such as filtration, centrifugation, reverse osmosis and the like are required to be carried out on the sample before chromatographic analysis, and the disposable porous medium adopted by the method can be directly used for loading actual samples such as river water, body fluid, petroleum and the like without any pretreatment. The porous medium can filter out most of suspended particles and relatively viscous and difficult-to-ionize substances in the actual sample.
(3) The porous medium is placed on the temperature control unit, and samples temporarily stored in small holes in the medium are sequentially desorbed from the medium according to the volatility sequence by slowly or rapidly increasing the temperature, so that dependence on expensive gas chromatograph and high performance liquid chromatograph in the prior analysis technology is eliminated, and dependence on gas chromatography equipment and liquid chromatography equipment is eliminated due to the fact that the gas chromatography technology and the liquid chromatography technology are avoided. The method provides a solution for the convenient and efficient online analysis of complex samples in common laboratories.
(4) The invention adopts the plasma discharge ion source (such as glow discharge ion source) to ionize the sample desorbed from the porous medium, and can realize the real-time online analysis of complex samples.
(5) The complex sample in the online analysis is a liquid dispersion system, and the real-time online analysis system for the complex sample can be suitable for real-time online detection of complex samples containing various components with gasification temperature lower than 500 ℃.
In the invention, the technical schemes can be mutually combined to realize more preferable combination schemes. Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and drawings.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, like reference numerals being used to refer to like parts throughout the several views.
FIG. 1 is a schematic diagram of a real-time online analysis system for complex samples in example 1;
FIG. 2 is an extracted ion flow chromatogram of each compound obtained by the real-time on-line analysis system of complex samples for analysis of urine samples of healthy adults in example 2;
FIG. 3 is an average mass spectrum obtained by the real-time on-line analysis system of complex samples of example 2 for analysis of urine samples of healthy adults;
reference numerals:
1-mass spectrum sample inlet; 2-a glow discharge ion source; 3-glass sand chip; 4-aluminum temperature control unit; 5-thermal resistance connection holes; 6-an alternating current power supply; 7-thermocouple connection holes; 8-a multimeter; 9-argon; 10 high voltage power supply interface.
Detailed Description
The invention provides a real-time online analysis system for complex samples, which comprises: a plasma discharge ion source; a temperature control unit; a disposable porous medium; the detection instrument is a mass spectrum.
The disposable porous medium is loaded with a sample in an analysis system, and under the heating of the temperature control unit, the components of the sample are dissipated and volatilized from the disposable porous medium at different speeds, so that the components gradually enter a sample inlet of a detection instrument to be detected. The disposable porous medium has the characteristic of low price. The disposable characteristic is that the disposable chromatographic column can be directly discarded after each use, so that the interference between samples is effectively avoided, and the chromatographic column is not required to be cleaned after the analysis of each sample is finished like the chromatographic-mass spectrometry technology. The steps and the flow are greatly saved, and the convenience of analysis and detection is improved.
Meanwhile, the research shows that the disposable porous medium has good filterability, liquid can escape and permeate on the disposable porous medium, but the solid is directly attached in the holes of the porous medium, so that the escape can not occur, the pretreatment flow before the measurement of the suspension and emulsion containing solid impurities is avoided, and the convenience of analysis and detection is improved. It should be noted that the disposable porous medium has the characteristic of large surface area, has adsorption effect on liquid, and meanwhile, the liquid has great surface tension in the porous medium, and has capillary action.
Specifically, the temperature control unit is in an aluminum cylindrical shape, has a diameter of 17-23mm and a thickness of 6-10mm, and is horizontally arranged at a position 3-7mm below the central axis of the mass spectrum sample inlet.
The diameter of the temperature control unit is not too large (not more than 23 mm), and the too large temperature control unit can generate thermal influence on the mass spectrum sample inlet and the ion source; because the temperature control unit provides heating for the porous medium, the temperature control unit with too small diameter can cause uneven self heating, and meanwhile, the temperature of the environment around the porous medium is unbalanced, so that the measurement is not facilitated. The temperature control unit is thus 17-23mm in diameter.
It should be noted that, the positions of the temperature control unit and the sample inlet need to be strictly controlled: the temperature control unit is horizontally arranged 3-7mm below the central axis of the mass spectrum sample inlet; if the distance is too large, the volatile substances dissipated by the porous medium cannot enter the mass spectrum for measurement due to too far ionization from the mass spectrum sample inlet, or only a small part of the substances enter the mass spectrum due to too far ionization, so that the measurement accuracy is affected; if the distance is too small, the upper surface of the porous medium is higher than the central axis of the mass spectrum sample inlet, so that the sample is directly dissipated and volatilized from the side edge of the porous medium without ionization and directly enters the mass spectrum, and the mass spectrum cannot detect the sample.
Specifically, the disposable porous medium is a glass sand chip for loading the sample.
The glass sand core is composed of excellent hard high-boron glass and has higher physical and chemical properties, the glass sand core is divided into six specifications of G1-G6 according to different pore diameters, and sand cores with different pore diameters can be attached and penetrated, so that the particle sizes of insoluble substances and properties (such as suspension, emulsion and colloid) in a sample to be detected are selected.
Specifically, the disposable porous medium is cylindrical, has a diameter of 4-6mm and a thickness of 3-5mm, and is placed on the upper surface of a platform of the temperature control unit. When the temperature control unit is cylindrical, one end face of the cylindrical disposable porous medium is arranged on the temperature control unit, namely, the two axes are parallel.
As described above, the porous medium has adsorption and capillary action, and in order to prevent the adsorption and capillary action from being uneven, substances having different adsorption capacities in the sample are volatilized and dissipated to the surface of the porous medium at the same time, so that a cylindrical porous medium must be selected. Meanwhile, the diameter of the porous medium is strictly controlled, and the diameter is 4-6mm; if the diameter of the porous medium is too small, capillary and adsorption effects are small, different substances are likely to be difficult to volatilize and dissipate to the surface of the porous medium in sequence due to the difference of the capillary and adsorption effects, and if the diameter of the porous medium is too large, the substances which volatilize and dissipate partially are ionized and then do not completely enter a mass spectrum sample inlet, so that measurement inaccuracy is caused. The thickness of the porous medium is limited in two ways: firstly, under the influence of the positions of a temperature control unit and a sample inlet, if the thickness is too small, a substance which is volatilized by the porous medium can not enter a mass spectrum for measurement due to too far ionization from the mass spectrum sample inlet, or only a small part of the substance enters the sample after the too far ionization, so that the measurement accuracy is affected, if the thickness is too large, the upper surface of the porous medium is higher than the central axis of the mass spectrum sample inlet, so that the sample is directly volatilized from the side edge of the porous medium without ionization, and directly enters the mass spectrum, and the mass spectrum can not detect the sample; secondly, if the thickness of the porous medium is too small, the capillary and adsorption effects of the porous medium and each component of the sample are small, so that different substances are likely to be difficult to volatilize and dissipate to the surface of the porous medium in sequence due to the difference of the capillary and adsorption effects, and if the thickness of the porous medium is too large, the substances which volatilize and dissipate partially are not completely introduced into a mass spectrum sample inlet after ionization, so that measurement inaccuracy is caused.
Specifically, two small holes are formed on the side surface of the temperature control unit, and are respectively used for placing a heating component (such as a thermal resistor connected with an alternating current power supply) and a temperature measuring element (such as a thermocouple connected with a universal meter). Specifically, the plasma discharge ion source is a glow discharge ion source, is placed above the temperature control unit, forms an included angle of 40-50 degrees with the horizontal plane, and is 2-5mm away from the central axis of the mass spectrum sample inlet at the tail end of the ion source, and is a glow discharge ion source plasma generation position. When the temperature control unit is in an aluminum cylindrical shape, the upper end face of the cylinder serves as a bearing platform of the temperature control unit, the disposable porous medium is placed on the bearing platform of the temperature control unit, the upper end face of the cylinder is parallel to the horizontal plane, at the moment, the central axis of the plasma discharge ion source and the bearing platform form an included angle of 40-50 degrees, and when the disposable porous medium is in a cylindrical shape, the central axis of the plasma discharge ion source and the upper end face of the cylindrical disposable porous medium form an included angle of 40-50 degrees.
After the mass spectrum is started up and self-inspected and enters a state to be sampled, the sample injector is in a vacuum state, when the temperature control unit starts heating, the mass spectrum sample inlet is opened, and sample molecules ionized by the ionization source are continuously sucked into the mass spectrum for measurement in the heating and ionization processes. Considering that too large an included angle between the plasma discharge ion source and the carrying platform of the temperature control unit causes insufficient ionization due to the action of air flow, too small an included angle causes uneven ionization due to the fact that the carrying platform is nearly parallel to the temperature control unit, experiments prove that a reasonable angle range is 40-50 degrees, and preferably 45 degrees.
It should be noted that, the end of the ion source should be controlled to be 2-5mm from the central axis of the mass spectrum sample inlet, the closer the end of the ion source is to the upper surface of the porous medium, the too close will cause the ionization source to ionize the sample molecules which are not volatilized and escaped from the upper surface of the porous medium together to cause the error of test data, meanwhile, the end of the ionization source has a certain temperature, the point heating can be carried out on the porous medium from the upper surface, the heating of the porous medium is changed, the volatilization and escaped sequence of the sample is changed, and the error of the measurement result is caused. The further the ion source end is from the mass spectrum sample inlet axis, the further the ion source end is from porous medium upper surface, and the too far can cause the ionization source unable to totally ionize the sample that the porous medium upper surface volatilized and dissipated, causes the inaccuracy of measured data.
Specifically, the glow discharge ion source uses argon as discharge gas, the direct-current high-voltage power supply provides high voltage, the discharge voltage and current can be regulated by the power supply, and the discharge gas size can be regulated by the gas rotameter.
The invention also provides a real-time online analysis system method for the complex sample, which comprises the following steps:
and 5, opening a sample inlet of the detection unit, and enabling all components in the sample to escape and volatilize from the load unit, and enabling the components to enter the detection unit for detection after being ionized by the ionization unit.
After the mass spectrum is started up for self-checking and enters a state to be sampled, an untreated actual liquid sample is dripped on the surface of a porous medium by using a syringe or a liquid shifter; the liquid sample on the surface of the porous medium is quickly infiltrated into the tortuous small holes in the porous medium for temporary storage due to the adsorption effect, the capillary effect and the gravity effect. The temperature control unit begins to rise in temperature and the porous medium and the liquid sample inside it are heated. The liquid sample is heated to evaporate and begins to escape in the order of volatility toward the upper surface of the porous medium. At the same time, the droplets in the porous medium are also subjected to capillary force of the small holes, adsorption action of the droplets and inner walls of the small holes, and resistance action of the tortuous pore channels on upward dissipation of the droplets. Under the combined influence of the actions, different substances in the mixture finally reach the surface of the porous medium at different times, and the substances volatilize and escape to the surface of the porous medium sequentially. However, suspended particles, colloid and the like in the original liquid sample stay in the pores in the porous medium and cannot escape to the outside of the porous medium. The atomized droplets separated from the surface of the porous medium are ionized by a plasma discharge ion source near a mass spectrum sample inlet to form ions, and the ions enter a mass spectrum in sequence to be detected under the action of negative pressure and an electric field.
Specifically, in the step 4, the temperature rising rate of the temperature control unit is 1.0-100.0 ℃/min.
The sample is heated to evaporate, capillary and adsorption in the porous medium and resistance of the tortuous channel. Under the combined influence of the actions, different substances in the mixture finally reach the surface of the porous medium at different times, and the substances volatilize and escape to the surface of the porous medium sequentially. Therefore, the slower the heating speed, the more fully the various acting forces act, and the larger the time difference between different substances reaching the surface of the porous medium, the more favorable the ionization and measurement are carried out sequentially. In order to realize real-time online analysis, the temperature rising rate is not too slow, so that the temperature rising rate of the temperature control unit is controlled to be-1.0-100.0 ℃/min.
Specifically, in step 4, qualitative analysis is performed through a mass spectrogram of the sample, and quantitative analysis is performed on the sample through drawing an extracted ion flow chromatogram.
Preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, which form a part hereof, and together with the description serve to explain the principles of the invention, and are not intended to limit the scope of the invention.
Example 1
The embodiment provides a real-time online analysis system for complex samples.
As shown in fig. 1, a glass sand chip 3 is used as a porous medium. The glass sand chip 3 has a diameter of 5mm and a thickness of 3mm, and is horizontally placed on an aluminum cylindrical temperature control unit 4 with a diameter of 20mm and a thickness of 8 mm. The temperature control unit is horizontally arranged at the position 5mm below the central axis of the mass spectrum sample inlet. Two small holes with the diameter of 2mm are formed in the side face of the aluminum temperature control unit 4 and are used for placing a thermal resistor (used for heating) connected with an alternating current power supply 6 and a thermocouple (used for measuring temperature) connected with a universal meter 8. Above the temperature control unit is placed a glow discharge ion source 2. The ion source forms an angle of 45 degrees with the horizontal plane, and the tail end of the ion source (the plasma generating place) is 3mm away from the central axis of the mass spectrum sample inlet. Argon 9 is used as discharge gas, and a direct current high-voltage power supply provides high voltage for a glow discharge ion source. The discharge voltage and current can be regulated by a power supply, and the discharge gas size can be regulated by a gas rotameter. The sample was added dropwise to the glass sand chip 3, and the liquid immediately infiltrated into the pores inside the meandering porous glass sand chip due to capillary action. And then an alternating current power supply is turned on to heat the temperature control platform. Due to the fact that the volatility of each component in the mixture sample is different, the size of non-covalent acting force of each component is different from that of small holes in the sand chip, and each component in the mixture is sequentially dissipated out of the surface of the glass sand chip along with the rising of temperature, so that separation is achieved. The glow discharge ion source 2 is turned on to ionize the sample that escapes from the surface of the glass sand chip while the alternating current power supply is turned on to heat. These samples are then sequentially detected by the action of negative pressure and electric field into the mass spectrum. The glass sand chip 3 is low in price, so that the glass sand chip is suitable for disposable use. The disposable sand chip avoids the interference between samples on one hand and provides a certain separation capability between different components of the same sample on the other hand.
Example 2
The embodiment provides a real-time online analysis method for complex samples, which is used for analyzing urine samples of healthy adults.
This example uses the complex sample real-time online analysis system described in example 1.
Urine samples contain about four thousand or more different compounds, with relatively high levels of urea, creatinine, and the like, and often mask the signals from other low levels of components. We herein analyze healthy adult urine samples with a mass spectrometry based complex sample real-time on-line analysis system. 10 microliters of urine sample without any pretreatment was taken and directly added dropwise to the surface of the glass sand chip. Then the heating power supply and the glow discharge ion source are turned on to start to analyze the compounds in the urine in sequence. In total more than 100 peaks were detected within an analysis time of 5 minutes total and m/z in the range 50-500. Fig. 2 shows an extracted ion flow chromatogram of several compounds commonly found in urine, and it can be seen that urea, creatinine and other compounds exhibit a distinct concentrated peak. For example, urea peaks at 0.9min and perillartine peaks around 1.4 min. Creatine, cysteine, arginine, creatinine and other compounds peak at about 2.0min,2.2min,2.8min and 3.7min, respectively. The concentration of the compound with higher content shows a peak, so that the interference to the measurement of other compounds with lower content is avoided. The concentration of compounds with lower content peaks, which corresponds to a single enrichment process, makes them easier to detect. FIG. 3 shows the mass spectrum of a urine sample detected by attributing several peaks with highest peak intensities (to increase ionization efficiency, derivatizing agent DMED was added to the urine sample, and the peaks detected here were at most [ M+DMED ] +.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention.
Claims (7)
1. The real-time online analysis system for the complex sample is characterized by comprising a load unit, a temperature control unit, an ionization unit and a detection unit;
the loading unit is a disposable porous medium and is used for loading a sample;
the temperature control unit is used for controlling the temperature of the sample loaded on the load unit;
the ionization unit is used for ionizing the sample which is volatilized out of the disposable porous medium;
the detection unit is a mass spectrometer and is used for carrying out qualitative and quantitative detection on the sample ionized by the ionization unit;
the disposable porous medium is a glass sand chip and is horizontally placed on the upper surface of the temperature control unit, the disposable porous medium is cylindrical, the diameter of the disposable porous medium is 4-6mm, and the thickness of the disposable porous medium is 3-5mm;
the temperature control unit has a heating rate of 1.0-100.0 ℃/min;
the temperature control unit is in a cylindrical shape made of aluminum, the diameter is 17-23mm, and the thickness is 6-10mm;
the ionization unit is placed above the load unit, and the tail end of the ionization unit is 2-5mm away from the central axis of the mass spectrum sample inlet.
2. The real-time online analysis system of a complex sample according to claim 1, wherein the ionization unit is a plasma discharge ion source.
3. The real-time online analysis system of complex samples according to claim 2, wherein the plasma discharge ion source is a glow discharge ion source.
4. The real-time on-line analysis system for complex samples according to claim 2, wherein the plasma discharge ion source forms an angle of 40-50 ° with the horizontal plane.
5. A real-time online analysis method of a complex sample, characterized in that the real-time online analysis system of a complex sample according to any one of claims 1 to 4 is used, comprising the steps of:
step 1, starting up the detection unit for self-checking, and entering a state to be sampled;
step 2, directly loading the sample to a load unit;
step 3, placing the load unit loaded with the sample on a platform of a temperature control unit;
step 4, starting the ionization unit, and heating up the temperature control unit at the same time;
and 5, opening a sample inlet of the detection unit, and enabling all components in the sample to escape and volatilize from the load unit, and enabling the components to enter the detection unit for detection after being ionized by the ionization unit.
6. The real-time online analysis method of complex samples according to claim 5, wherein in the step 4, the temperature rising rate of the temperature control unit is 1.0-100.0 ℃/min.
7. The real-time online analysis method of complex samples according to claim 5, wherein in step 5, qualitative analysis is performed by mass spectrogram of the samples, and quantitative analysis is performed on the samples by drawing extracted ion flow chromatograms.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011260649.9A CN114460213B (en) | 2020-11-10 | 2020-11-10 | Real-time online analysis system and method for complex sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011260649.9A CN114460213B (en) | 2020-11-10 | 2020-11-10 | Real-time online analysis system and method for complex sample |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114460213A CN114460213A (en) | 2022-05-10 |
| CN114460213B true CN114460213B (en) | 2023-06-20 |
Family
ID=81404811
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011260649.9A Active CN114460213B (en) | 2020-11-10 | 2020-11-10 | Real-time online analysis system and method for complex sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114460213B (en) |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5078456B2 (en) * | 2007-06-19 | 2012-11-21 | キヤノン株式会社 | Mass spectrometry substrate, mass spectrometry method, and mass spectrometer |
| CN103021786B (en) * | 2012-12-24 | 2015-10-28 | 复旦大学 | A kind of Filter-type electrospray ionization source device for mass spectral analysis |
| CN103901145A (en) * | 2014-04-08 | 2014-07-02 | 四川大学 | Normal-pressure micro-glow discharge desorption mass spectrum ion source and mass spectrometry device composed of ion source |
| CN104007168B (en) * | 2014-06-09 | 2016-06-01 | 中国科学院上海有机化学研究所 | A kind of sample carrier for ionization massspectrum analysis and application thereof |
| CN104237371B (en) * | 2014-09-11 | 2017-01-11 | 上海应用技术学院 | Simple device for realizing real-time direct injection analysis of mass spectrometer and application of simple device |
| CN105513934B (en) * | 2014-09-25 | 2017-12-19 | 中国科学院大连化学物理研究所 | A kind of layering Thermal desorption sample injection method for ion mobility spectrometry |
| CN107664660B (en) * | 2017-09-15 | 2020-10-23 | 清华大学深圳研究生院 | Sample target for mass spectrometry, preparation method thereof and mass spectrometry method |
| CN108152360B (en) * | 2018-02-08 | 2020-12-11 | 中国检验检疫科学研究院 | Dielectric barrier discharge ionization mass spectrometry analysis method for perfluorinated compounds in textiles |
| CN109192652B (en) * | 2018-08-24 | 2019-12-10 | 山东省分析测试中心 | Mass spectrum detection method of sulfonate genotoxic impurities based on dielectric barrier discharge ion source |
| CN210037730U (en) * | 2019-05-29 | 2020-02-07 | 中国科学院化学研究所 | Mass spectrum analysis device |
-
2020
- 2020-11-10 CN CN202011260649.9A patent/CN114460213B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN114460213A (en) | 2022-05-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Moldoveanu et al. | Essentials in modern HPLC separations | |
| Lundanes et al. | Chromatography: basic principles, sample preparations and related methods | |
| Lord et al. | Evolution of solid-phase microextraction technology | |
| Engelhardt | High performance liquid chromatography | |
| Hubschmann | Handbook of GC-MS: fundamentals and applications | |
| Hamilton | Ion exchange chromatography of amino acids. A single column, high resolving, fully automatic procedure. | |
| WO2012029303A1 (en) | Device for preparing sample supplied to ion mobility sensor | |
| Tu et al. | Determination of mercury species by capillary zone electrophoresis-inductively coupled plasma mass spectrometry: a comparison of two spray chamber–nebulizer combinations | |
| CN107561151B (en) | Quick pesticide residue detector based on mass spectrometry technology | |
| CN103323543B (en) | Method for detecting 17 polycyclic aromatic hydrocarbons in cigarette gas | |
| Li | Rapid speciation analysis of mercury by short column capillary electrophoresis on-line coupled with inductively coupled plasma mass spectrometry | |
| Guo et al. | Solid-phase microextraction combined with electrochemistry | |
| Tian et al. | Movable reduction bed hydride generation system as an interface for capillary zone electrophoresis and inductively coupled plasma atomic emission spectrometry for arsenic speciation analysis | |
| Zhang et al. | In‐capillary solid‐phase extraction–capillary electrophoresis for the determination of chlorophenols in water | |
| Cody et al. | Coated glass capillaries as SPME devices for DART mass spectrometry | |
| CN114460213B (en) | Real-time online analysis system and method for complex sample | |
| Zhang et al. | A miniature optical emission spectrometric system in a lab-on-valve for sensitive determination of cadmium | |
| Zhang et al. | Sandwich-type spontaneous injection of nitrophenols for capillary electrophoresis analysis | |
| JP3654715B2 (en) | Method for quantitative analysis of silicone oil | |
| CN114093748A (en) | Compact structure's photoionization ion source and photoionization time of flight mass spectrograph | |
| RU2523765C1 (en) | Photo-ionisation detector for gas analysers | |
| CN112986219A (en) | Electrode sample introduction DBD micro plasma atomic emission spectrum detection system and method | |
| Wenhu et al. | Determination of trace volatile organic compounds in water samples by membrane introduction mass spectrometry | |
| Drabik et al. | Hyphenated techniques | |
| RU2229122C1 (en) | Procedure establishing summary content of hydrocarbons in analyzed mixture |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |