CN109781473A - A kind of negative ion mobility spectrometry detection method of propofol in exhaled breath - Google Patents
A kind of negative ion mobility spectrometry detection method of propofol in exhaled breath Download PDFInfo
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- CN109781473A CN109781473A CN201711114399.6A CN201711114399A CN109781473A CN 109781473 A CN109781473 A CN 109781473A CN 201711114399 A CN201711114399 A CN 201711114399A CN 109781473 A CN109781473 A CN 109781473A
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- 229960004134 propofol Drugs 0.000 title claims abstract description 37
- OLBCVFGFOZPWHH-UHFFFAOYSA-N propofol Chemical compound CC(C)C1=CC=CC(C(C)C)=C1O OLBCVFGFOZPWHH-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000001514 detection method Methods 0.000 title claims abstract description 13
- 238000001871 ion mobility spectroscopy Methods 0.000 title claims description 15
- 238000005070 sampling Methods 0.000 claims abstract description 65
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 53
- 238000001228 spectrum Methods 0.000 claims abstract description 17
- 239000012159 carrier gas Substances 0.000 claims description 61
- 239000007789 gas Substances 0.000 claims description 48
- 150000002500 ions Chemical class 0.000 claims description 44
- 230000005012 migration Effects 0.000 claims description 28
- 238000013508 migration Methods 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 238000012546 transfer Methods 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 12
- 238000004458 analytical method Methods 0.000 claims description 10
- 230000009471 action Effects 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 230000002285 radioactive effect Effects 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 239000002808 molecular sieve Substances 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 3
- 150000001450 anions Chemical class 0.000 abstract description 28
- 238000010790 dilution Methods 0.000 abstract description 19
- 239000012895 dilution Substances 0.000 abstract description 19
- 238000012544 monitoring process Methods 0.000 abstract description 8
- 230000003595 spectral effect Effects 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 description 17
- 230000005611 electricity Effects 0.000 description 4
- 238000009791 electrochemical migration reaction Methods 0.000 description 4
- 206010002091 Anaesthesia Diseases 0.000 description 3
- 230000037005 anaesthesia Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- -1 Propofol ion Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000001990 intravenous administration Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a kind of anions of Propofol in expiratory air to migrate spectrum detection method.Spectral technology is migrated based on time resolution dynamic dilution sampling device and reagent molecule auxiliary photo-ionisation anion, realize the time resolution dynamic dilution sample introduction of propofol molecule and hydrone in expiratory air, eliminate the influence of humidity and other chaff interferents in expiratory air, it is quantitative to it by the maximum signal of time resolution dynamic dilution sample introduction 4s Propofol, realize the clinical continuous on-line monitoring of Propofol in expiratory air.
Description
Technical field
The present invention is based on time resolution dynamic dilution sampling devices and reagent molecule to assist photo-ionisation anion migration spectrum, if
A kind of ionic migration spectrum detection method for having counted time resolution dynamic dilution sample introduction realizes Propofol and expiratory air in expiratory air
The time resolution dynamic dilution sample detection of middle humidity, eliminates the influence of humidity in expiratory air, utilizes sample introduction 4s Propofol
Signal strength it is quantitative to it, realize the continuous on-line monitoring of Propofol in expiratory air.
Background technique
Propofol is a kind of common Intravenous Anesthesia agent, and existing more than 50 a countries are used at present.It, can in surgical procedure
The Anesthesia Monitoring leaned on is the important leverage of patient vitals' safety, and existing research shows to monitor on-line the third pool in patient's expiratory air
Phenol concentration is expected to become a kind of noninvasive, online Anesthesia Monitoring means.
Ion mobility spectrometry (Ion Mobility Spectrometry, IMS) is a kind of atmosphere risen the 1970s
Gaseous ion isolation technics under the conditions of pressure provides a kind of simple, quick, highly sensitive analysis means for expiratory air.However,
For ion mobility spectrometry, humidity interference is a serious problem, it can both reduce the sensitivity and selectivity of measurement, and
And it also will increase the complexity of spectrogram, and then substantially reduce the accuracy of result.Therefore, for the expiratory air sample of high humidity, often
The input mode of rule is worthless for ion mobility spectrometry.In current application study, usually by more bundles of capillaries
Column (MCC) or film sampling device are combined with ion mobility spectrometry, utilize the pre-separation ability of MCC or the hydrophobicity of film sampling device
To achieve the purpose that eliminate humidity interference.But due to the combination of MCC and film sampling device, so that the response time of IMS is up to
Minute grade, cannot achieve the real time on-line monitoring of expiratory air.
The present invention provides a kind of detection methods of Propofol in clinical continuous on-line monitoring expiratory air, utilize reagent molecule
It assists photo-ionisation anion to migrate spectral technology, eliminates the interference of other chaff interferents, binding time differentiates dynamic dilution sample introduction dress
It sets, different with adsorptivity of the humidity in tetrafluoro sampling ring using the Propofol in expiratory air, hydrone, which first dilutes, to be come out, the third pool
Dilution comes out after phenol, eliminates the influence of humidity in expiratory air, the method does not need any sample pre-treatments, realizes expiratory air
The continuous on-line monitoring of the clinic of middle Propofol.
Summary of the invention
The present invention migrates spectral technology by using reagent molecule auxiliary photo-ionisation anion, and binding time differentiates dynamic dilution
Sampling device eliminates the influence of humidity and other chaff interferents in expiratory air, and the clinic for realizing Propofol in expiratory air is continuous
On-line monitoring.
The anion of Propofol migrates spectrum detection method in a kind of expiratory air, is divided into following two step:
1) sampling process, sample gas is stored in sampling ring under the action of sampling pump, and carrier gas is directly entered ion at this time
Migration tube, sampling time 10-20s；
2) sample introduction process, sampling pump stop working, and sample carrier gas at this time flows through sampling ring and send sample molecule therein
Enter in transference tube and detected, in the process, for the concentration of each compound by dynamic dilution, sample molecule is first in sampling ring
Afterwards enter ionic reaction area, react with the reagent ion in transference tube reaction zone, generation product ion, by migration area according to
Secondary separation reaches Faraday plate and is detected, sample injection time 10-15s.
Wherein, expiratory air 16 is connected through flow sensor 15 with the interface A of the first two-position three way magnetic valve 14 by pipeline,
The interface B of first two-position three way magnetic valve 14 is connect with the Single port of sampling ring 17, the another port of sampling ring 17 and the two or two
The interface A connection of position-3-way solenoid valve 13, the interface B of the second two-position three way magnetic valve 13 are connect with 18 air inlet of sampling pump；Sample
Product carrier gas inlet 11 is connect by pipeline with the interface A of third two-position three way magnetic valve 12, third two-position three way magnetic valve 12
Interface B is connect by pipeline with anion mobility spectrometer air inlet；The interface C of third two-position three way magnetic valve 12 and the two or two
The interface C connection of three-way magnetic valve 13；The interface C of first two-position three way magnetic valve 14 by pipeline and anion mobility spectrometer into
Port connection；
Reagent molecule carrier gas 8 enters pipeline, the pipeline and the first two-position three way electricity by reagent molecule generating device 10
Pipeline, 12 interface B of third two-position three way magnetic valve and anion between the interface C and anion mobility spectrometer air inlet of magnet valve 14
Pipeline between mobility spectrometer air inlet is interconnected；
When sampling, expiratory air 16 passes through flow sensor 15, the 1st three by pipeline under the action of sampling pump 18
14 interface A of three-way electromagnetic valve, 14 interface B of the first two-position three way magnetic valve, sampling ring 17,13 interface A of the second two-position three way magnetic valve,
Second two-position three way magnetic valve, 13 interface B, sampling pump 18；
Sample carrier gas is through sample carrier gas inlet 11 by pipeline through third two-position three way magnetic valve interface A, the three or two three
12 interface B of three-way electromagnetic valve and anion mobility spectrometer air inlet enter transference tube；Organic agent molecule carrier gas 8 passes through pipeline
Enter transference tube through reagent molecule generating device 10 and anion mobility spectrometer air inlet；Sampling time 10-20s；
When sample introduction, switch three solenoid valves while sampling pump 18 stops, sample carrier gas is passed through through sample carrier gas inlet 11
12 interface A of third two-position three way magnetic valve, 12 interface C of third two-position three way magnetic valve, 13 interface of the second two-position three way magnetic valve
C, 13 interface A of the second two-position three way magnetic valve, sampling ring 17,14 interface B of the first two-position three way magnetic valve, the first two-position three way electricity
14 interface C of magnet valve enters anion migration spectrum；Organic agent molecule carrier gas 8 through reagent molecule generating device 10 and is born by pipeline
Ionic migration spectrometer air inlet enters transference tube；
Sampling ring 17 is the four fluorine tube (outer diameter 4mm, internal diameter 3mm) of long 150cm, the hollow volume with 10.6ml, temperature
It is constant in 25-30 DEG C of range.
The ion mobility spectrometry is the anion migration spectrum that reagent molecule assists photo-ionisation, and the light ionization source 1 used is non-
Radioactive vacuum UV lamp, the lamp are low pressure Kr gas discharge lamp (the Kr10.6-B12X50PID lamp, Steven of commercialization
Sepvest Corporation), the main photon for generating 10.0eV and 10.6eV, light intensity is about 5 × 1011Photons/s,
The photon intensity that the photon intensity of middle 10.0eV accounts for 80%, 10.6eV accounts for 20%.
Ion mobility spectrometry includes the transference tube with Faraday plate receiving pole, and the transference tube close to Faraday plate moves
It moves area one end and is equipped with drift gas entrance 7, transference tube reaction zone one end far from Faraday plate is equipped with total gas outlet 9, in drift gas
End of the transference tube in the reaction zone of migration area between entrance 7 and total gas outlet 9, the entrance equipped with sample carrier gas；
End of the transference tube in the reaction zone of migration area between drift gas entrance 7 and total gas outlet 9, is equipped with
The air inlet of organic agent molecule carrier gas stream is carried, organic agent molecule enters reaction zone by air inlet；
The entrance of the sample carrier gas and the air inlet of organic agent molecule carrier gas stream are same air inlet, and setting is being floated
End of the transference tube in the reaction zone of migration area between gas entrance (7) and total gas outlet (9).
Organic agent molecule used by ion mobility spectrometry is acetone.
The power supply of on-radiation vacuum UV lamp used in reagent molecule auxiliary photo-ionisation anion migration spectrum is
Radio-frequency power supply.
Sample carrier gas is consistent with reagent molecule carrier gas stream direction in reaction zone, consistent with migration area drift gas airflow direction；
All gas in transference tube leaves transference tube by total gas outlet.
The sample carrier gas, reagent molecule carrier gas and to float the gas of gas be through in active carbon, silica gel or molecular sieve
The filtered air of one or more.
Reagent molecule air inlet and sample carrier gas air inlet are at 0 ° of -180 ° of angle on transference tube.
The concentration of organic agent molecule is 10-20ppm in gas of carrier gas containing organic agent molecule.
Advantages of the present invention:
The present invention is filled using reagent molecule auxiliary photo-ionisation anion migration spectral technology and time resolution dynamic dilution sample introduction
It sets, eliminates humidity in expiratory air and other materials interference, realize the continuous online prison of clinic of Propofol in expiratory air
It surveys.
Detailed description of the invention
Fig. 1, the structural schematic diagram of time resolution dynamic dilution sampling device and transference tube that this method is related to, 1 is
Vacuum UV lamp ionization source, 2 be Bradbury-Nielsen, and 3 be conducting ring, and 4 be aperture plate, and 5 be signal amplifier, 6 be-
5000V high pressure, 7 be drift gas entrance, and 8 be reagent molecule carrier gas, and 9 be total gas outlet, and 10 be reagent molecule generating device, and 11 be sample
Product carrier gas inlet 12 is third two-position three way magnetic valve, 13 be the second two-position three way magnetic valve, 14 be the first two-position three-way electromagnetic
Valve, 15 be flow sensor, and 16 be expiratory air, and 17 be tetrafluoro sampling ring, and 18 be aspiration pump.
Fig. 2, when reagent molecule is acetone, the ion transfer spectrogram of 1ppbv Propofol under 0%RH and 100%RH；
Fig. 3, when reagent molecule is acetone, the time resolution dynamic dilution sample introduction 10s process of 1ppbv Propofol under 0%RH
Ion transfer spectrogram；
Fig. 4, when reagent molecule is acetone, the time resolution dynamic dilution sample introduction 10s mistake of 1ppbv Propofol under 100%RH
The ion transfer spectrogram of journey；
Fig. 5, when reagent molecule is acetone, the dynamically track spectrogram of 1ppbv Propofol peak height under 0%RH and 100%RH.
Specific embodiment
The invention discloses a kind of ionic migration spectrum detection methods of Propofol in expiratory air, using reagent molecule fill-in light
It ionizes anion and migrates spectral technology, binding time differentiates dynamic dilution sampling device, eliminates humidity and other objects in expiratory air
The interference of matter realizes the detection of Propofol in expiratory air.
Sampling process, sample gas is stored in sampling ring under the action of sampling pump, and carrier gas is directly entered ion and moves at this time
Move pipe, sampling time 20s.
Sample introduction process, sampling pump stop working, and sample carrier gas at this time flows through sampling ring and is sent into sample molecule therein
It is detected in transference tube, in the process, for the concentration of each compound by dynamic dilution, sample molecule is successive in sampling ring
It into ionic reaction area, is reacted with the reagent ion in transference tube reaction zone, generates product ion, successively by migration area
Separation reaches Faraday plate and is detected, sample injection time 10s.
Wherein, expiratory air 16 is connected through flow sensor 15 with the interface A of the first two-position three way magnetic valve 14 by pipeline,
The interface B of first two-position three way magnetic valve 14 is connect with the Single port of sampling ring 17, the another port of sampling ring 17 and the two or two
The interface A connection of position-3-way solenoid valve 13, the interface B of the second two-position three way magnetic valve 13 are connect with 18 air inlet of sampling pump；Sample
Product carrier gas inlet 11 is connect by pipeline with the interface A of third two-position three way magnetic valve 12, third two-position three way magnetic valve 12
Interface B is connect by pipeline with anion mobility spectrometer air inlet；The interface C of third two-position three way magnetic valve 12 and the two or two
The interface C connection of three-way magnetic valve 13；The interface C of first two-position three way magnetic valve 14 by pipeline and anion mobility spectrometer into
Port connection；
Reagent molecule carrier gas 8 enters pipeline, the pipeline and the first two-position three way electricity by reagent molecule generating device 10
Pipeline, 12 interface B of third two-position three way magnetic valve and anion between the interface C and anion mobility spectrometer air inlet of magnet valve 14
Pipeline between mobility spectrometer air inlet is interconnected；
When sampling, expiratory air 16 passes through flow sensor 15, the 1st three by pipeline under the action of sampling pump 18
14 interface A of three-way electromagnetic valve, 14 interface B of the first two-position three way magnetic valve, sampling ring 17,13 interface A of the second two-position three way magnetic valve,
Second two-position three way magnetic valve, 13 interface B, sampling pump 18；
Sample carrier gas is through sample carrier gas inlet 11 by pipeline through third two-position three way magnetic valve interface A, the three or two three
12 interface B of three-way electromagnetic valve and anion mobility spectrometer air inlet enter transference tube；Organic agent molecule carrier gas 8 passes through pipeline
Enter transference tube through reagent molecule generating device 10 and anion mobility spectrometer air inlet；
When sample introduction, switch three solenoid valves while sampling pump 18 stops, sample carrier gas is passed through through sample carrier gas inlet 11
12 interface A of third two-position three way magnetic valve, 12 interface C of third two-position three way magnetic valve, 13 interface of the second two-position three way magnetic valve
C, 13 interface A of the second two-position three way magnetic valve, sampling ring 17,14 interface B of the first two-position three way magnetic valve, the first two-position three way electricity
14 interface C of magnet valve enters anion migration spectrum；Organic agent molecule carrier gas 8 through reagent molecule generating device 10 and is born by pipeline
Ionic migration spectrometer air inlet enters transference tube；
The ion mobility spectrometry is the anion migration spectrum that reagent molecule assists photo-ionisation, and the light ionization source 1 used is non-
Radioactive vacuum UV lamp, the lamp are low pressure Kr gas discharge lamp (the Kr10.6-B12X50PID lamp, Steven of commercialization
Sepvest Corporation), the main photon for generating 10.0eV and 10.6eV, light intensity is about 5 × 1011Photons/s,
The photon intensity that the photon intensity of middle 10.0eV accounts for 80%, 10.6eV accounts for 20%.
Ion mobility spectrometry includes the transference tube with Faraday plate receiving pole, and the transference tube close to Faraday plate moves
It moves area one end and is equipped with drift gas entrance 7, transference tube reaction zone one end far from Faraday plate is equipped with total gas outlet 9, in drift gas
End of the transference tube in the reaction zone of migration area between entrance 7 and total gas outlet 9, equipped with entering for sample carrier gas
Mouthful；
End of the transference tube in the reaction zone of migration area between drift gas entrance 7 and total gas outlet 9, is equipped with
The air inlet of organic agent molecule carrier gas stream is carried, organic agent molecule enters reaction zone by air inlet, and sample carrier gas enters
Mouth and organic agent molecule air inlet are same entrance.
Organic agent molecule used by ion mobility spectrometry is acetone.
The power supply of on-radiation vacuum UV lamp used in reagent molecule auxiliary photo-ionisation anion migration spectrum is
Radio-frequency power supply.
Sample carrier gas is consistent with reagent molecule carrier gas stream direction in reaction zone, consistent with migration area drift gas airflow direction；
All gas in transference tube leaves transference tube by total gas outlet.
The sample carrier gas, reagent molecule carrier gas and to float the gas of gas be through in active carbon, silica gel or molecular sieve
The filtered air of one or more.
The air inlet of reagent molecule and the air inlet of sample carrier gas are at 0 ° of angle on transference tube.
The concentration of organic agent molecule is 15ppm in carrier gas containing organic agent molecule.
Embodiment 1
Photo-ionisation anion migration spectrum is assisted using reagent molecule, binding time differentiates the detection of dynamic dilution sampling device
1ppbv Propofol under 0%RH and 100%RH, when wherein reagent molecule is acetone, as shown in Fig. 2, the reduction of reagent ion migrates
Rate is 2.31cm2V-1s-1, under 0%RH under 1ppbv Propofol and 100%RH 1ppbv Propofol ion transfer spectrogram, Propofol
The reduction mobility of product ion is 1.37cm2V-1s-1。
As shown in figure 3, the ion mobility spectrometry under 0%RH during 1ppbv Propofol time resolution dynamic dilution sample introduction 10s
Figure, in the 6s of sample introduction process, Propofol dilutes out, and reaches maximum signal.
As shown in figure 4, the Ion transfer under 100%RH during 1ppbv Propofol time resolution dynamic dilution sample introduction 10s
Spectrogram, the difference of the adsorptivity in tetrafluoro sampling ring due to propofol molecule in expiratory air and hydrone, before sample introduction process
3s, the hydrone in expiratory air, which first dilutes, to be come out, and 4s Propofol dilutes out, and reaches maximum signal, to eliminate
The influence of humidity in expiratory air.
As shown in figure 5, under 0%RH and 100%RH 1ppbv Propofol peak height dynamically track spectrogram, 6 times repetition detect,
Wherein, the relative standard deviation of Propofol is that the relative standard deviation of Propofol under 0.96%, 100%RH is under 0%RH
0.81%, preferably, the humidity in expiratory air utilizes Propofol during sample introduction 10s under 100%RH close to 100%RH to repeatability
Maximum signal the Propofol in expiratory air is quantified.
Claims (10)
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Cited By (1)
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