CN106645770A - An on-line detector capable of continuous sample injection and application thereof - Google Patents
An on-line detector capable of continuous sample injection and application thereof Download PDFInfo
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- CN106645770A CN106645770A CN201510736090.5A CN201510736090A CN106645770A CN 106645770 A CN106645770 A CN 106645770A CN 201510736090 A CN201510736090 A CN 201510736090A CN 106645770 A CN106645770 A CN 106645770A
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- thermal desorption
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Abstract
An on-line detector capable of continuous sample injection is designed in the invention. According to the detector, an ion-mobility spectrometry technique as a base detection technique is adopted and sample thermal desorption analysis and headspace sample feeding techniques are combined. A sample with a complex matrix does not need pretreatment and is collected to the surface of a sampling sheet, the sampling sheet allows volatile components of the sample to be gasified in a thermal desorption analysis sample injector through a belt type conveying manner, and then the sample vapor is carried by a carrier gas to enter the detector and subjected to on-line detection and analysis. The detector achieves on-line continuous detection of propofol in human blood during operations and is used for directing clinical administration by doctors.
Description
Technical field
The present invention is based on Ion mobility spectrometry, with reference to sample Thermal desorption and headspace sampling technology, design
A kind of continuous sample introduction on-line detector.Detection means and method in the present invention is used for third in blood
Pool phenol clinical administration depth analysis, instruct the accurate medication of clinical anesthesia doctor.
Background technology
Thermal desorption technology is a kind of two in one technique:Collection sampling with concentrate in one, then by sample from
Detected after being transferred out in sampling pipe.Dynamic headspace analysis are also referred to as purge ＆ trap, and the method is
Fluid sample (or surface of solids) is passed through with inert gas, the component to be analyzed is purged out, be allowed to
It is enriched with by a container for filling adsorbent, then adsorbent is heated again, is made adsorbed
Component is desorbed, and is brought in gas chromatographic column with carrier gas and is analyzed.
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 occur with molecule, obtains multi-products ion.Ion
The ion gate opened by periodicity under the ordering about of electric field enters migration area, the neutral drift gas with adverse current
Molecule is continually colliding, because these ions have in the electric field different migration rates so that different
Ion separated, successively reach detector.The present invention is based on Ion mobility spectrometry, with reference to sample
Product Thermal desorption and headspace sampling technology, devise a kind of on-line detector of continuous sample introduction.This detection dress
Put is used for Propofol clinical administration depth analysis in blood with method, realizes continuous sample introduction analysis.
The content of the invention
A kind of on-line detector of continuous sample introduction, including sampling device and ionic migration spectrometer；Sample introduction is filled
Put including Thermal desorption room, heater, ribbon sampling cloth and roller.
Thermal desorption room be closed container, in closed container bottom be provided with one as thief hatch through hole；In
Be provided with a transparent glass platform below thief hatch, thief hatch in platform projection in the plane be located at
On platform, the lower section of platform is connected with the output shaft of motor, is driven by motor flat
Platform pumps in through hole lower section along the axial direction of through hole；Heating lamp is fixed with below platform, plus
The light that thermolamp sends is exposed in Thermal desorption room by clear glass window, and heating lamp provides Thermal desorption heat
Source；In Thermal desorption room upper end be provided with one as sample inlet through hole, sample inlet be located at thief hatch just
Top；Ribbon sampling cloth is laid between thief hatch and push rod platform, the two ends of ribbon sampling cloth
It is wound in respectively on roller；
In Thermal desorption room top and/or side wall be provided with carrier gas inlet and carrier gas outlet；Carrier gas inlet with
Carrier gas source of the gas is connected, and carrier gas outlet is connected with the carrier gas air inlet of ion mobility spectrometry detector migration tube
It is logical.
There are ribbon sampling cloth, the two ends winding of ribbon sampling cloth in the middle of Thermal desorption room and heater
On roller or it is pressed between roller and roller fixed mount, rotates to change by roller and be located at Thermal desorption room
Thermal desorption sample introduction region；There is heating Halogen lamp LED Thermal desorption room lower end, there is provided Thermal desorption thermal source.
Rolling sampling cloth is the polytetrafluoroethylene (PTFE) high temperature samples cloth or all-glass paper of strip, and highest is resistant to
500℃。
The roller is connected with the output shaft of motor, drives roller to rotate by the output shaft of motor；By
Motor allows sampling cloth to carry out crawler type transmission motion, and motion process is：Sampling cloth can be with continuous sampling reality
When monitor detection signal.
Transparent glass platform is held sampling cloth and is adopting sampling cloth pinch seal with Thermal desorption room on heating lamp
At sample mouth, now sample Jing Thermal desorptions room upper end sample inlet enters the corresponding sampling in Thermal desorption room bottom
On cloth.
Sample instills sampling cloth, and Thermal desorption room is in air-tight state, and heating lamp is turned on light 1-10S, is now carried
Gas carries headspace sample steam and sends into the analysis detection of ion mobility spectrometry migration tube.
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.
On-line detector recited above is used in blood in the detection process of Propofol, realizes blood
The continuous sample introduction analysis of middle Propofol sample.
Advantages of the present invention is as follows：
1. compared with traditional chromatographic process, using the detector in the present invention as the hand for analyzing sample
Section has advantages below：Complex matrices sample is without the need for special pre-treatment, it is possible to achieve continuous online inspection
Survey.
2. detection speed is fast, greatlys save analysis time, and the single sample testing time is less than 1min；
3. the operating cost of apparatus is low, and running stores are few；The cost performance of instrument is high, without the need for specialty
Background human users.
Description of the drawings
Fig. 1 is continuous sample introduction on-line detector apparatus structure principle schematic；
In figure：1 is sampling device, 2 is transference tube, 3 is blood sample conduit, 4 is pyrolysis
Analysis room, 5 be heat power supply device, 6 be electric rotating machine, 7 be rolling sampling sheet, 8 be carrier gas inlet, 9 be
Thermal desorption room sample inlet, 10 be the carrier gas outlet of Thermal desorption room or sample gas enter migration tube inlet, 11
For migration tube ionized region, 12 be ion gate, 13 be migration tube migration area, 14 be aperture plate, 15 to put
Big device, 16 be A/D converter, 17 be data acquisition processing system, 18 be for drift gas entrance, 19
Gas outlet, 20 are ion receiving pole.
Specific embodiment
Continuous sample introduction on-line detector is shown in Fig. 1 using traditional uniform field migration spectrum, its structural representation.
This instrument mainly includes following components：1 is sampling device, 2 is transference tube, 3 is blood
Sample line, 4 be Thermal desorption room, 5 be heat power supply device, 6 be electric rotating machine, 7 be rolling sampling cloth,
8 be carrier gas inlet, 9 be sample inlet, 10 be carrier gas outlet or sample gas enter migration tube inlet, 11
For migration tube ionized region, 12 be ion gate, 13 be migration tube migration area, 14 be aperture plate, 15 to put
Big device, 16 be A/D converter, 17 be data acquisition processing system, 18 be for drift gas entrance, 19
Gas outlet, 20 are ion receiving pole.
Flow controller is connected with blood sample conduit 3, sample injection volume is controlled, heat power supply device 5 is
Heat by lalonge lamp provides the endogenous pyrogen of Thermal desorption room 4；The upper brace support of heat power supply device 5 sampling cloth seals heat
Resolution Room bottom；After sample introduction, light irradiation 1-10S is heated；Carrier gas Jing carrier gas inlets 8 carry head space pyrolysis
Gassing body enters analysis detector and is analyzed by transference tube air inlet 10.Complete above-mentioned once to divide
After analysis detection, electric rotating machine 6 drives rolling sampling cloth 7 to change Thermal desorption sample introduction region.New sampling
Cloth enters Thermal desorption room position directly below, pending analysis detection next time.
Carrier gas and drift gas source of the gas adopt the Medical air (air) of purified treatment, and carrier gas in test
400sccm, floats gas 600sccm.
The on-line detector of continuous sample introduction is used for into propofol agent in blood according to above-mentioned implementation process
Detection.
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 9ms.In blood concentration 1-10ng/ μ L concentration range build-in tests, testing standard curve side
Journey simultaneously calculates detection sensitivity.The continuous sample introduction on-line detector adopted in the present invention can obtain standard
Curve linear correlation is more than 0.99, detection sensitivity 0.2ng/ μ L.
This apparatus is used for the detection of propofol agent clinic blood concentration, meets Clinical practice need
Ask.For the apparatus and method that the accurate medication of Anesthetist provides complete set.
Claims (7)
1. a kind of on-line detector of continuous sample introduction, it is characterised in that：Move including sampling device and ion
Move spectrometer；Sampling device includes Thermal desorption room, heater, ribbon sampling cloth and roller；
Thermal desorption room be closed container, in closed container bottom be provided with one as thief hatch through hole；In
Be provided with a transparent glass platform below thief hatch, thief hatch in platform projection in the plane be located at
On platform, the lower section of platform is connected with the output shaft of motor, is driven by motor flat
Platform pumps in through hole lower section along the axial direction of through hole；Heating lamp is fixed with below platform, plus
The light that thermolamp sends is exposed in Thermal desorption room by clear glass window, and heating lamp provides Thermal desorption heat
Source；In Thermal desorption room upper end be provided with one as sample inlet through hole, sample inlet be located at thief hatch just
Top；Ribbon sampling cloth is laid between thief hatch and push rod platform, the two ends of ribbon sampling cloth
It is wound in respectively on electric rotating machine roller；
In Thermal desorption room top and/or side wall be provided with carrier gas inlet and carrier gas outlet；Carrier gas inlet with
Carrier gas source of the gas is connected, and carrier gas outlet is connected with the carrier gas air inlet of ion mobility spectrometry detector migration tube
It is logical.
2. on-line detector according to claim 1, it is characterised in that：Thermal desorption room and heating
The two ends for having ribbon sampling cloth, ribbon sampling cloth in the middle of device are wrapped on roller or are pressed in rolling
Between wheel and roller fixed mount, rotated by roller and changed positioned at the Thermal desorption sample introduction region of Thermal desorption room；
There is heating Halogen lamp LED Thermal desorption room lower end, there is provided Thermal desorption thermal source.
3. on-line detector according to claim 1 and 2, it is characterised in that：Rolling sampling cloth
For the polytetrafluoroethylene (PTFE) high temperature samples cloth or all-glass paper of strip, highest is resistant to 500 DEG C.
4. on-line detector according to claim 1 and 2, it is characterised in that：The roller with
The output shaft of motor is connected, and drives roller to rotate by the output shaft of motor；Entered by sampling sheet by motor
The transmission of journey belt is moved, and motion process is：Sampling cloth can be with continuous sampling real-time monitoring detection signal.
5. on-line detector according to claim 1, it is characterised in that：Transparent glass on heating lamp
Glass platform holds sampling cloth and Thermal desorption room by sampling cloth pinch seal at thief hatch, now sample Jing
Thermal desorption room upper end sample inlet is entered on the corresponding sampling cloth in Thermal desorption room bottom.
6. on-line detector according to claim 1, it is characterised in that：Sample instills sampling cloth,
Thermal desorption room is in air-tight state, and heating lamp is turned on light 1-10S, and now carrier gas carries headspace sample steam and send
Enter the detection of Ion transfer analysis of spectrum.
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.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510736090.5A CN106645770A (en) | 2015-11-03 | 2015-11-03 | An on-line detector capable of continuous sample injection and application thereof |
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| CN201510736090.5A CN106645770A (en) | 2015-11-03 | 2015-11-03 | An on-line detector capable of continuous sample injection and application thereof |
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Cited By (5)
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|---|---|---|---|---|
| CN109470547A (en) * | 2017-09-07 | 2019-03-15 | 中国科学院大连化学物理研究所 | A kind of gradient pyrolysis analysis sample injector |
| CN110873753A (en) * | 2018-08-30 | 2020-03-10 | 中国科学院大连化学物理研究所 | Enrichment method for separating gas-phase free propofol in whole blood sample |
| CN111999132A (en) * | 2019-09-05 | 2020-11-27 | 中国科学院大连化学物理研究所 | Aerosol sampling analyzer |
| CN112577781A (en) * | 2020-12-10 | 2021-03-30 | 中国科学院大连化学物理研究所 | Thermal analysis device for aerosol sampling of linear conversion adsorption sheet |
| CN112945656A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院大连化学物理研究所 | Simple and portable online enrichment device and method |
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| CN110873753B (en) * | 2018-08-30 | 2022-05-31 | 中国科学院大连化学物理研究所 | Enrichment method for separating gas-phase free propofol in whole blood sample |
| CN111999132A (en) * | 2019-09-05 | 2020-11-27 | 中国科学院大连化学物理研究所 | Aerosol sampling analyzer |
| CN112945656A (en) * | 2019-12-11 | 2021-06-11 | 中国科学院大连化学物理研究所 | Simple and portable online enrichment device and method |
| CN112577781A (en) * | 2020-12-10 | 2021-03-30 | 中国科学院大连化学物理研究所 | Thermal analysis device for aerosol sampling of linear conversion adsorption sheet |
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