CN106645367A - Online detector combining ultrasonic atomization and ion mobility spectrometry and application - Google Patents

Online detector combining ultrasonic atomization and ion mobility spectrometry and application Download PDF

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Publication number
CN106645367A
CN106645367A CN201510736073.1A CN201510736073A CN106645367A CN 106645367 A CN106645367 A CN 106645367A CN 201510736073 A CN201510736073 A CN 201510736073A CN 106645367 A CN106645367 A CN 106645367A
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China
Prior art keywords
ultrasonic atomizatio
ultrasonic
room
piece
line detector
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CN201510736073.1A
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李海洋
李恩有
王新
王祯鑫
渠团帅
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/622Ion mobility spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention designs an online detector combining ultrasonic atomization and ion mobility spectrometry. According to the detector, an ion mobility spectrometry technology is adopted as a basic detection technology and is combined with an ultrasonic atomization technology for samples. A blood sample is collected to the surface of a sampling piece without pretreatment, and then, the sample is turned into a fine mist drop state with the ultrasonic atomization technology and carried into the detector by the aid of carrier gas for online detection analysis. The online detector is applied to online detection of propofol in human blood in an operation and can guide a doctor in clinical administration.

Description

A kind of on-line detector and application of ultrasonic atomizatio in combination with ion mobility spectrometry
Technical field
The present invention is based on Ion mobility spectrometry, with reference to sample ultrasonic atomization and headspace sampling technology, if A kind of on-line detector is counted.Detection means and method in the present invention is used to into Propofol in blood to face Bed administration depth analysis, instruct the accurate medication of clinical anesthesia doctor.
Background technology
Using electronics high frequency oscillation, (frequency of oscillation is 1.7MHz or 2.4MHz to ultrasonic atomizer, is exceeded The audibility range of people, the electronic is to human body and animal fanout free region), by the high frequency of ceramic atomizing piece Resonance, aqueous water minor structure is broken up and the elegant water smoke of nature is produced, and is not required to heat or add appoint What chemical reagent.Compare with heating atomization mode, energy saving 90%.
Propofol is a kind of conventional Intravenous Anesthesia agent, and anesthesia induction, anesthesia dimension have been widely used in Hold and ICU for heavy patient calmness.In surgical procedure, the concentration of propofol in patient blood is often There is close correlation with its depth of anesthesia, therefore the concentration of Propofol in patient blood is monitored in art Have great importance for Anesthesia Monitoring.
Being presently used for determining the method for Propofol in blood mainly includes that high performance liquid chromatography and makings join With etc..However, biological sample of the blood as a complexity, necessary before it carries out chromatographic isolation Sample pretreatment is carried out, so as to cause above method time-consuming longer, and mostly off-line analysis, it is impossible to it is complete The demand of full up foot clinically Anesthesia Monitoring.
Ion mobility spectrometry (Ion Mobility Spectrometry, IMS) technology is 20th century 70 A kind of quick separating detection technique that age occurs, compared with traditional mass spectrum, chromatographic apparatus, has Simple structure, sensitivity is high, and analyze speed is fast, the characteristics of reliable results.The IMS that at present we study Be widely used in chemical warfare agent, drugs, explosive detection, environmental monitoring, monitoring poisonous gas, The fields such as fire monitoring, water pollution monitoring and food inspection.Ionic migration spectrometer mainly by ion gun, Ion gate, migration area and detector composition.Ion gun makes sample molecule, N2、O2Ionize with vapor, The ion of generation is easy to that ion molecule reaction occurs with molecule, obtains multi-products ion.Ion exists The ion gate opened by periodicity under the ordering about of electric field enters migration area, the neutral drift gas point with adverse current Son is continually colliding, because these ions have in the electric field different migration rates so that different Ion is separated, and successively reaches detector.The present invention is based on Ion mobility spectrometry, with reference to sample Ultrasonic atomizatio and headspace sampling technology, devise a kind of on-line detector.
The content of the invention
A kind of on-line detector of ultrasonic atomizatio in combination with ion mobility spectrometry, including sampling device and from Sub- mobility spectrometer;Sampling device includes ultrasonic atomizatio room, ultrasonic atomizer and takes blood sampling sheet and ultrasound Atomizing piece;
Ultrasonic atomizatio room be a closed container, its upper end be provided with one as fluid sample entrance through hole, Fluid sample entrance is provided with dismountable closure;Ultrasonic atomizatio room is respectively arranged on the left side and the right side a through hole, One is carrier gas inlet, another for carrier gas gas outlet, and ultrasonic atomizatio piece is placed with ultrasonic atomizatio room, Ultrasonic atomizatio piece top is placed with sampling sheet, and the ultrasonic atomizatio outdoor below ultrasonic atomizatio piece is provided with Ultrasonic atomizer, i.e. ultrasonic atomizer are arranged at the lower section of ultrasonic atomizatio room;Fluid sample entrance is located at Sampling sheet top;
Carrier gas inlet is connected with carrier gas source of the gas, the carrier gas air inlet phase of carrier gas outlet and transference tube Connection.
Bottom in ultrasonic atomizatio room is provided with a groove, has ultrasonic atomizatio in the bottom surface tiling of groove Piece;Sampling sheet is placed in ultrasonic atomizatio piece top, and sampling sheet is mutually amplexiformed with ultrasonic atomizatio piece.
Ultrasonic atomizatio room bottom is by ultrasonic atomizatio room sealed bottom by a dismountable dividing plate;Every Plate upper surface is provided with a groove, and the surface tiling ultrasonic atomizatio piece in groove, sampling sheet is placed in ultrasound Atomizing piece top;
3-8 root springs are uniformly provided with dividing plate lower section, spring lower section sets support, spring and the side of support one Ultrasonic atomizer is fixed in face, on the other hand by the flexible realizing opening and closing ultrasonic mist of spring Change the dividing plate of room bottom.
Fluid sample entrance is provided with dismountable closure, and when sample is added dropwise closure is opened, and this leads to Open in hole;Closure is closed when ultrasonic atomizatio and headspace sampling process, this through hole is closed;
Sample is done after the pre-treatment of ultrasonic atomizatio head space again using the principle of ultrasonic atomizatio for sampling device Sample introduction is analyzed.
Sampling sheet is the polytetrafluoroethylene (PTFE) high temperature samples cloth or glass consistent with ultrasonic atomizatio piece size shape Fibrous paper;Designed size is generally the wafer architecture of diameter 1-3cm.
When ultrasonic atomizer works, ultrasonic atomizatio piece is driven during sampling sheet concussion, ultrasonic atomizatio room Bottom baffles are set on state, it is to avoid the interference that ultrasonic vibration brings, after concussion process terminates, Ultrasonic atomizatio room bottom baffles are set to off closed state, carry out headspace sampling analysis.
On-line detector in the present invention is used in blood in the detection process of propofol agent.Blood The ultrasonic atomizatio time control of liquid sample is in 1-10S.
Transference tube includes ionized region, ion gate, migration area, the grid sequentially coaxially arranged in housing Net and ion receiving pole;Drift gas entrance is provided near the housing sidewall of ion receiving pole, gas entrance is floated It is connected with drift gas source of the gas;Housing sidewall between ion gate and ionization source is provided with gas vent, should Gas vent is vented.
The present invention is based on Ion mobility spectrometry, with reference to ultrasonic atomizatio and headspace sampling technology, devises A kind of on-line detector, is used for the detection means and method in the present invention Propofol clinic in blood and gives Medicine depth analysis, improve the detection sensitivity of Propofol in blood.
Advantages of the present invention is as follows:
1. compared with traditional gas chromatography, using the detector in the present invention as analysis sample Means there is advantages below:Fluid sample can be without the need for the direct ultrasound in injector of complicated pre-treatment Atomization, it is possible to achieve fluid sample on-line checking;
2. sampling device is simple, and analysis detection speed is fast, and the single sample testing time is less than 1min; The operating cost of instrument is low, and running stores are few;
3. the sampling device that detector is combined in the present invention saves energy without the need for electrical heating Thermal desorption technology Source.
Description of the drawings
Fig. 1 is the on-line detector apparatus structure principle schematic in the present invention;1 be microsyringe, 2 is silica gel tightening nut (containing " O " circle), 3 is ultrasonic atomizatio room, 4 is to take blood sampling sheet and ultrasound Atomizing piece, 5 be ultrasonic atomizer, 6 be carrier gas inlet, 7 be carrier gas outlet, 8-15 be migration tube knot Structure;8 be sample gas enter migration tube inlet, 9 be migration tube ionized region, 10 be ion gate, 11 be Migration tube migration area, 12 be aperture plate, 13 be ion receiving pole, 14 for drift gas entrance, 15 be outlet Mouthful.
Specific embodiment
Using traditional uniform field migration spectrum, its structural representation is shown in Fig. 1 to Propofol in blood.This instrument Mainly include following components:1 is microsyringe, 2 is silica gel tightening nut (containing " O " circle), 3 be ultrasonic atomizatio room, 4 for take blood sampling sheet and ultrasonic atomizatio piece, 5 be ultrasonic atomizer, 6 to carry Gas entrance, 7 are that carrier gas is exported, 8-15 is migration tube structure;8 be sample gas enter migration tube inlet, 9 be migration tube ionized region, 10 be ion gate, 11 be migration tube migration area, 12 be aperture plate, 13 be from Sub- receiving pole, 14 are gas outlet for drift gas entrance, 15.
Cavity lower surface is amplexiformed with the structure of ultrasonic atomizer outer chamber upper surface two outside ultrasonic atomizatio room, It is internally formed the cavity of a sky;There is silica gel tightening nut at ultrasonic atomizatio room upper surface center (containing " O " Circle) can open, sample is instilled by microsyringe.Bottom in ultrasonic atomizatio room be provided with one it is recessed Groove, has ultrasonic atomizatio piece in the bottom surface tiling of groove;Sampling sheet is placed in ultrasonic atomizatio piece top, and adopts Print is mutually amplexiformed with ultrasonic atomizatio piece.Ultrasonic atomizer bottom below ultrasonic atomizatio room is by one Dismountable dividing plate is by ultrasonic atomizatio room sealed bottom.3-8 root springs are uniformly provided with dividing plate lower section, Spring lower section sets support, and on the one hand spring and support are fixed ultrasonic atomizer, on the other hand by bullet The flexible dividing plate to realize opening and closing ultrasonic atomizatio room bottom of spring.
Using operating procedure to open the upper end tightening nut 2 of ultrasonic atomizatio room 3, taken with microsyringe 1 Blood sample Jing ultrasonic atomizatios room upper end through hole is added dropwise on the sampling sheet 4 of ultrasonic atomizatio room bottom;So Afterwards ultrasonic atomizer stretches dividing plate by support, and control dividing plate does not contact ultrasonic atomizatio chamber room lower limb, Then ultrasonic atomizatio piece 1-10S, then moment closing ultrasonic atomizatio room are started.Carrier gas Jing carrier gas inlets 6 are taken With the headspace sample gas after ultrasonic atomizatio transference tube air inlet 8 is entered by transference tube by 7 (8-15) it is analyzed detection.
After completing above-mentioned once analysis detection, ultrasonic atomizer appliance stand spring is compressed, more renewed The pending analysis detection next time of sampling sheet.
Carrier gas and drift gas source of the gas adopt the source of the gas (air) of purified treatment, and carrier gas in test 400sccm, floats gas 600sccm, and source of the gas humidity is 0-20ppm.
On-line detector by ultrasonic atomizatio in combination with ion mobility spectrometry is used for according to above-mentioned implementation process The detection of propofol agent in blood.
Propofol injection drug standards are taken, concentration is 10000ng/ μ L;It is dilute step by step with blank plasma Release, be configured to blood concentration be 1,2.5,5,7.5, the sample of 10ng/ μ L, it is standby.Single mark The testing result of quasi- sample, when reagent ion peak transit time is in 6ms, the detection of Propofol standard is moved Shift time is in 9.5ms.In blood concentration 1-10ng/ μ L concentration ranges, testing standard curvilinear equation And calculate detection sensitivity.The on-line detector adopted in the present invention can improve detection sensitivity 5-10 times.
This apparatus is used for into the detection of propofol agent clinic blood concentration, Clinical practice is met Demand.A set of new apparatus and method are provided for the accurate medication of Anesthetist.

Claims (8)

1. on-line detector of a kind of ultrasonic atomizatio in combination with ion mobility spectrometry, it is characterised in that:Bag Include sampling device and ionic migration spectrometer;Sampling device includes ultrasonic atomizatio room, ultrasonic atomizer and adopts Print;
Ultrasonic atomizatio room be a closed container, its upper end be provided with one as fluid sample entrance through hole, Fluid sample entrance is provided with dismountable closure;Ultrasonic atomizatio room is respectively arranged on the left side and the right side a through hole, One is carrier gas inlet, another for carrier gas gas outlet, and ultrasonic atomizatio piece is placed with ultrasonic atomizatio room, Ultrasonic atomizatio piece top is placed with sampling sheet, and the ultrasonic atomizatio outdoor below ultrasonic atomizatio piece is provided with Ultrasonic atomizer, i.e. ultrasonic atomizer are arranged at the lower section of ultrasonic atomizatio room;Fluid sample entrance is located at Sampling sheet top;
Carrier gas inlet is connected with carrier gas source of the gas, the carrier gas air inlet phase of carrier gas outlet and transference tube Connection.
2. on-line detector according to claim 1, it is characterised in that:In ultrasonic atomizatio room Bottom be provided with a groove, in groove bottom surface tiling have ultrasonic atomizatio piece;Sampling sheet is placed in ultrasound Above atomizing piece, and sampling sheet is mutually amplexiformed with ultrasonic atomizatio piece.
3. on-line detector according to claim 1 and 2, it is characterised in that:Ultrasonic atomizatio room Bottom is by ultrasonic atomizatio room sealed bottom by a dismountable dividing plate;Dividing plate upper surface is provided with one Individual groove, the surface tiling ultrasonic atomizatio piece in groove, sampling sheet is placed in ultrasonic atomizatio piece top;
3-8 root springs are uniformly provided with dividing plate lower section, spring lower section sets support, spring and the side of support one Ultrasonic atomizer is fixed in face, on the other hand by the flexible realizing opening and closing ultrasonic mist of spring Change the dividing plate of room bottom.
4. on-line detector according to claim 1, it is characterised in that:
Fluid sample entrance is provided with dismountable closure, and when sample is added dropwise closure is opened, and this leads to Open in hole;Closure is closed when ultrasonic atomizatio and headspace sampling process, this through hole is closed;
Sample is done after the pre-treatment of ultrasonic atomizatio head space again using the principle of ultrasonic atomizatio for sampling device Sample introduction is analyzed.
5. on-line detector according to claim 1, it is characterised in that:Sampling sheet is and ultrasound The consistent polytetrafluoroethylene (PTFE) high temperature samples cloth of atomizing piece size shape or all-glass paper;Designed size one As for diameter 1-3cm wafer architecture.
6. on-line detector according to claim 3, it is characterised in that:Ultrasonic atomizer works When, ultrasonic atomizatio piece is driven during sampling sheet concussion, and ultrasonic atomizatio room bottom baffles are set on State, it is to avoid the interference that ultrasonic vibration brings, after concussion process terminates, ultrasonic atomizatio room bottom baffles Closed state is set to off, headspace sampling analysis is carried out.
7. the application of the arbitrary on-line detector of a kind of claim 1-6, it is characterised in that:It is described On-line detector is used in blood in the detection process of propofol agent.
8. the application of on-line detector according to claim 7, it is characterised in that:Blood sample Ultrasonic atomizatio time control is in 1-10S.
CN201510736073.1A 2015-11-03 2015-11-03 Online detector combining ultrasonic atomization and ion mobility spectrometry and application Pending CN106645367A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109839421A (en) * 2017-11-27 2019-06-04 中国科学院大连化学物理研究所 The method quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid
CN110208358A (en) * 2019-05-21 2019-09-06 暨南大学 A kind of high-frequency vibration atomization ionization probe device and method
CN111220678A (en) * 2018-11-23 2020-06-02 中国科学院大连化学物理研究所 Ion mobility spectrometer
CN112086339A (en) * 2019-06-13 2020-12-15 中国科学院大连化学物理研究所 Ultrasonic atomization sample injector for ion mobility spectrometry

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005172692A (en) * 2003-12-12 2005-06-30 National Institute For Agro-Environmental Science Trace liquid continuous atomization device and standard gas generation device using it
CN103884771A (en) * 2012-12-21 2014-06-25 中国科学院大连化学物理研究所 Accurate method for detecting propofol anesthetic in blood
CN104716001A (en) * 2013-12-13 2015-06-17 中国科学院大连化学物理研究所 Liquid continuous sampling device for heating and gasification

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005172692A (en) * 2003-12-12 2005-06-30 National Institute For Agro-Environmental Science Trace liquid continuous atomization device and standard gas generation device using it
CN103884771A (en) * 2012-12-21 2014-06-25 中国科学院大连化学物理研究所 Accurate method for detecting propofol anesthetic in blood
CN104716001A (en) * 2013-12-13 2015-06-17 中国科学院大连化学物理研究所 Liquid continuous sampling device for heating and gasification

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109839421A (en) * 2017-11-27 2019-06-04 中国科学院大连化学物理研究所 The method quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid
CN111220678A (en) * 2018-11-23 2020-06-02 中国科学院大连化学物理研究所 Ion mobility spectrometer
CN110208358A (en) * 2019-05-21 2019-09-06 暨南大学 A kind of high-frequency vibration atomization ionization probe device and method
CN112086339A (en) * 2019-06-13 2020-12-15 中国科学院大连化学物理研究所 Ultrasonic atomization sample injector for ion mobility spectrometry
CN112086339B (en) * 2019-06-13 2021-06-15 中国科学院大连化学物理研究所 Ultrasonic atomization sample injector for ion mobility spectrometry

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Application publication date: 20170510