CN106198702A - A kind of method of drugs in quick detection saliva - Google Patents
A kind of method of drugs in quick detection saliva Download PDFInfo
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- CN106198702A CN106198702A CN201510226674.8A CN201510226674A CN106198702A CN 106198702 A CN106198702 A CN 106198702A CN 201510226674 A CN201510226674 A CN 201510226674A CN 106198702 A CN106198702 A CN 106198702A
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Abstract
The invention discloses a kind of method of drugs in quick detection saliva.Take saliva sample and add aqueous slkali regulation pH value, then measure above-mentioned saliva solution at sample introduction sheet sampling, then in saliva sample, add the assistant chemical additive of certain volume, sample introduction sheet is sent in ion migration analysis of spectrum detector Thermal desorption injector.Testing result is analyzed through the detection output of Thermal desorption post analysis.Measure detection limit and can reach below 1ng magnitude (below 0.1ppm concentration).Single sample is less than 5S, software automatic output detections result analysis time.Measuring method simplicity, quick, efficient, good reliability in the present invention.Enter to take poison for mouth, case of taking drugs, ion migration analysis of spectrum detector utilizes the method in the present invention can realize quickly inspection by drug ingredient in detection saliva completely.Based on the applied research demand in terms of forensic science, software controls instrument can implement alarm mode according to drugs migration time.
Description
Technical field
The invention discloses a kind of method of drugs in quick, sensitive detection saliva, with ion migration
Spectral technology is basic detection technique, uses positive and negative ion pattern, establishes ion mobility spectrometry and quickly examine
Survey the qualitative method of drugs in saliva.In recent years, drugs are increasing to the harm of human lives,
Orthobiosis through serious threat to the mankind.So the detection to drugs is extremely important, particularly suck
The confirmation of drugs people's crime fact.This measuring method is easy, quick, efficient, good reliability.For
Mouth enters to take poison, case of taking drugs, and ion mobility spectrometry can be realized by drug ingredient in detection saliva completely
Rapid screening.
Background technology
Saliva is a kind of colourless and thin liquid, is commonly called as saliva by people, although claimed in ancient times
For " Jinin good wine ", the most always there are unclean indecency sense in the modern times to people.By three pairs of major salivary glands (lower jaws
Gland, rib gland and sublingual gland) mucus of many little mucus glands secrete on the liquid secreted and oral cavity wall, at mouth
The Digestive system mixed in chamber.Saliva colorless and odorless, PH is 6.6 to 7.1.Normal person secretes every day
Amount be about 1.0 to 1.5 liters (herbivore such as cattle, sheep, every day salivation amount up to body weight 1/3).
In the saliva of people, 99% is water.
In recent years, by research saliva, people find that again saliva has multiple new purposes.
Diagnose the illness: body generation pathological changes, necessarily make the chemical analysis of saliva change the most therewith.
Having only to dry saliva generate crystallization, crystal shape is different with pathological changes, thus can serve as diagnosis
Evidence such as hypertension, parotitis, cholera, diabetes, ascariasis etc..
Diseases prevention gives protection against cancer: the compositions such as the mucin in saliva can neutralize part gastric acid, produces precipitation, attachment
On gastric mucosa, form protective layer, peptic ulcer can be prevented and treated.Additionally, bacteriolyze contained in saliva
Enzyme, can not only kill or suppress staphylococcus, Bacillus typhi, escherichia coli, Hemolytic streptococcus etc.,
But also the carcinogenic toxicity such as flavacin benzopyrene, nitrosamine can be made to be substantially reduced, even become
Innocuous substance.
Monitoring medication: after medication, gather saliva within a certain period of time, chemically examine its drug content, just
May know that this medicine concentration in blood.
The optimum utilization of saliva is to find disease.Studying now saliva reflection and osteoporosis,
Disorder of hormone secretion and arteriosclerosis, the contact especially and between the lethal disease such as acquired immune deficiency syndrome (AIDS).Expert
Pointing out, saliva is the active substance of the noxious substances such as detection drugs.
The kind of drugs is divided into according to abuse route: is administered orally, aspirates or injects.Different drugs are to people
Injury be also different, its lethal mechanism is the most different.Heroin, is commonly called as " white lead ".It is to use
A kind of drugs of coffee synthesis.As morphine, respiratory center is had extremely strong inhibitory action.And white lead
Effect is 5 times of morphine.Excess can cause heart beating the most slow, dyspnea and dead.Cocaine, ancient
The alkaloid that Ke Yezhong extracts.Central nervous system there is very toxic.Excess is sucked can stimulate bone marrow,
Cause respiratory failure and dead.Methamphetamine and derivant thereof, be commonly called as ice, and primary raw material is
Ephedrine.Damaged brain function, causes heart failure.Its derivant is novel amfetamine, namely
Dancing outreach.Infringement cardiovascular system and central nervous system.Excessive use causes palpitating speed, blood pressure
Rise and cause to set out internal hemorrhage and dead.The drugs quickly analyzed in detection saliva are the most very important
A difficult problem.Ketamine (English: ketamine), is commonly called as KET, KET, KET, KET, is
The drugs of mental department (drugs) of a kind of danger close, belongs to Anesthesia Department of non-Opium system medicine.Daily seen
The Main Ingredients and Appearance of ketamine product is ketalar, and chemical formula is C13H16ClNO HCl, molecule
Amount is 274.19.It is white powdered solid substance under normal temperature and pressure.Fusing point is 266 degree,
Noninflammability.PH value 3.5～5.5, aqueous solution is acidity.
In recent years, drugs are increasing to the harm of human lives, and the number of drug abuse is in the whole world day by day
Increasing, the situation of drug smuggling is increasingly severe, and illicit drugs inspection field is increasingly becoming important field.
The chemical method such as high performance liquid chromatography, immunoassay is the method that comparison is traditional.These methods are all
Having their respective limitation, such as higher to detection environmental requirement, the detection cycle is long etc..
Ion mobility spectrometry (Ion Mobility Spectrometry, IMS) technology 20 century 70 occurs
A kind of separation detection technique, compared with traditional mass spectrum, chromatographic apparatus, has simple in construction, sensitive
Degree height, analyzes speed fast, the feature of reliable results.In atmospheric environment, trace substance can be carried out
Detection, is suitable to onsite application.Therefore this technology can be applied to the on-line checking of precursor chemicals.
Summary of the invention
It is an object of the invention to provide and a kind of utilize ion mobility spectrometry quickly to detect the side of drugs in saliva
Method.In order to realize direct, quick, the sensitive detection of drugs in saliva, the technology that the present invention uses
Scheme is:
1) drugs Standard analysis tests: take 10-100 μ L drugs standard substance and drip to correspondence on sample introduction sheet
At sampling, then coupongs are sent in ion mobility spectrometry Thermal desorption injector.Respectively at ion mobility spectrometry
Carry out detection under positive ion mode to analyze, it is thus achieved that each Autonomous test signal；Determine drugs under positive ion mode
Go out peak migration time；
2) saliva sample analysis test: accurately measure 100-500 μ L saliva sample, first add alkali
Between solution (sodium carbonate or sodium bicarbonate) regulation pH value 8.5-9.5, then measure 10-50 μ L
Above-mentioned saliva solution, at sample introduction sheet sampling, adds the auxiliary of 1-10 times of volume in saliva sample simultaneously
Chemical addition agent, then sample introduction sheet is sent in ion migration analysis of spectrum detector Thermal desorption injector.Point
Under ion mobility spectrometry positive ion mode, do not carry out detection analyze, it is thus achieved that each Autonomous test signal；According to it
Sample peak migration time and the step 1 obtained) in spectrogram storehouse drugs signal peak migration time contrast, enter
And whether determine in saliva containing Poison？
In the aqueous slkali regulation pH value method of above-mentioned addition certain volume, the alkali liquor volume of addition is equal to saliva
The sample volume of liquid sample, alkali liquor refers to sodium carbonate or sodium bicarbonate aqueous solution.
Sodium carbonate or sodium bicarbonate aqueous solution concentration are 2*10-8.5mol/L to 2*10-9.5mol/L
Between.
When sample introduction sheet sample detection is analyzed, add auxiliary Thermal desorption chemical addition agent methanol, second simultaneously
Alcohol or acetonitrile, can be greatly improved detection sensitivity.
Auxiliary Thermal desorption chemical addition agent, auxiliary Thermal desorption chemical addition agent is blended in one with saliva sample
Rising, described chemical addition agent is anhydrous reagent, and addition is 1-10 times of saliva sample sampling volume.
Method in the present invention can detect respectively be suitable for the oral or drugs Opium of suction, heroin,
Morphine, Fructus Cannabis, cocaine, head-shaking pill, methamphetamine hydrochloride, dolantin, KET, cherry chestnut, Opium, caffeine,
Amphetamines, methylene dioxygen methamphetamine
Advantages of the present invention is as follows:
1. ion mobility spectrometry is as drugs analysis means in saliva, it is possible to achieve on-the-spot in situ, the fastest
Speed is analyzed.
The most whole instrument total amount is less than 10kg, and instrument compact is portable, easy to carry, and instrument is independent
Run, be suitable for onsite application；
3. measuring speed is fast；There is no the sample pre-treatments test of complexity, be especially suitable for on-site quick screening；
The operating cost of instrument is the lowest, and consumable goods is little；The cost performance of instrument is high, analyzes alarm velocity 5
In second.
4. this measuring method regulation saliva PH value and assistant chemical additive can be greatly improved detection sensitive
Degree: the method in the present invention can make detection sensitivity improve 1 order of magnitude；The purpose of tune pH value is
Strengthen drugs dissolubility in saliva.Add assistant chemical additive purpose is to promote drugs pyrolysis simultaneously
Gassing, and then improve detection sensitivity.
Accompanying drawing explanation
Fig. 1 is the ion mobility spectrometry apparatus structural principle schematic diagram of drugs in detection saliva；
1 is ionized region, and 2 is migration area, and 3 is Thermal desorption injector, and 4 is gas-carrier pipeline, and 5 is ion
Source, 6 is gas outlet, and 7 is ion gate, and 8 is migration ring in migration tube, and 9 is aperture plate, and 10 is drift gas
Pipeline, 11 is detector；
Fig. 2 is ion mobility spectrometry background signal ion migration spectrogram (RIP) under positive ion mode；
Fig. 3 be under positive ion mode ion mobility spectrometry detection KET content be 100ppm saliva sample from
Son migrates spectrogram；
Detailed description of the invention
In following example, the operation of involved ion mobility spectrometry all uses the ion of structure shown in Fig. 1 to move
Move spectral apparatus to detect；Following example intermediate ion migrates the experiment condition of spectrum and is: ionization source is
Radioactivity63The ion mobility spectrometry in Ni source, motor injector.During experiment, migration tube temperature is maintained at
100 DEG C, injector temperature 180 DEG C, carrier gas (air), drift gas (air) air-flow be respectively 400,
600mL/min.Saliva sample containing drugs is after Thermal desorption heating devices heat, and drugs add with auxiliary
Agent volatilize together sample introduction analysis detection.
In order to realize quick, the Sensitive Detection of drugs in saliva, present invention ion mobility spectrometry is as dividing
Every kind of drugs standard substance are dissolved in organic solvent (being made into the solution of 1-1000ppm) by analysis means respectively,
As calibrating reagent sample, drip to respectively on sample introduction sheet with ionic migration spectrometer be in the positive-ion mode
Detecting instrument, obtains detection signal respectively, the migration of the different drugs of input in detector software system
Temporal information, sets up drugs standard substance ion migration analysis of spectrum testing result spectrogram storehouse, and software identification is moved
Shifting rate information is the detection of drugs in testing sample.
Embodiment 1
Air background detects:
The blank sampling sheet not adding any sample is sent into ion migration analysis of spectrum detector Thermal desorption
In injector.The temperature of Thermal desorption injector is at 180 DEG C.The sample gas that Thermal desorption obtains is (empty by carrier gas
Gas, with injector resolution temperature 180 DEG C) bring the ionized region of ion mobility spectrometry into, the flow of carrier gas exists
400sccm；Sample is ionized to positive and negative ion at ionized region, by the ion gate periodically opened,
Enter the drift region being made up of uniform electric field, obtain in drift region separating and detection acquisition instrumental background inspection
Survey signal.Fig. 2 gives the ion mobility spectrometry with positive ion mode ion mobility spectrometry detection air background
Figure, it can be seen that positive ion mode reagent ion peak (RIP) occurs about at 4.36ms.
Embodiment 2
Saliva background detection:
The method utilizing the present invention to provide utilizes the process of the blank saliva sample of ion mobility spectrometry detection such as
Under: take saliva sample, add sodium bicarbonate aqueous solution (2*10-9Mol/L) regulation pH value is 9, so
After measure the 50 above-mentioned saliva solution of μ L at sample introduction sheet sampling, the body such as interpolation in saliva sample simultaneously
Long-pending assistant chemical additive ethanol, then sample introduction sheet is sent into ion migration analysis of spectrum detector Thermal desorption
In injector.The temperature of Thermal desorption injector is at 180 DEG C.The sample gas that Thermal desorption obtains is (empty by carrier gas
Gas, with injector resolution temperature 180 DEG C) bring the ionized region of ion mobility spectrometry into, the flow of carrier gas exists
400sccm；Sample is ionized to positive and negative ion at ionized region, by the ion gate periodically opened,
Enter the drift region being made up of uniform electric field, obtain in drift region separating and detection.Under positive ion mode
Saliva detection signal also only has air reagent ion peak (RIP) to occur in about 4.36ms, and saliva is carried on the back
Scape is without other signal disturbing.
Embodiment 3
The detection of drugs in saliva sample:
Utilize the process of ketamine (KET) in ion mobility spectrometry detection saliva as follows:
(1) drugs Standard analysis tests: by ketamine (KET), Opium is dissolved in respectively 95% second
Alcoholic solvent, is made into the solution of 100-500ppm respectively；Two kinds of solution carry out ion migration analysis of spectrum respectively
Detection, obtains detection signal respectively, sets up drugs standard substance ion mobility spectrometry with the detection signal obtained
Analyze testing result spectrogram storehouse；Particularly as follows: take above-mentioned KET solution 1 μ L to drip to ion migration analysis of spectrum
At sampling corresponding on the sample introduction sheet of detector, then coupongs are sent into ion mobility spectrometry Thermal desorption sample introduction
In device, under ion mobility spectrometry positive ion mode, carry out detection analyze；Take above-mentioned Opium solution repeat with
Upper operation, two kinds of solution each obtain detection signal, determine that under positive ion mode, the peak that goes out of drugs migrates
Time；Revising ion migration analysis of spectrum testing result spectrogram storehouse, wherein the migration time of KET is
5.88ms, the migration time 9.36ms of Opium.Above ion mobility spectrometry analysis condition is: Thermal desorption
The temperature of injector is at 180 DEG C.(air, with injector solution by carrier gas for the sample gas that Thermal desorption obtains
Eutectoid temperature 180 DEG C) bring the ionized region of ion mobility spectrometry into, the flow of carrier gas is at 400sccm.
(2) saliva sample analysis test: take saliva sample (containing KET 100ppm), adds bicarbonate
Sodium water solution (2*10-9Mol/L) regulation pH value 9, then measure the 50 above-mentioned saliva solution of μ L in
At sample introduction sheet sampling, in saliva sample, add isopyknic assistant chemical additive ethanol simultaneously, then
Sample introduction sheet is sent in ion migration analysis of spectrum detector Thermal desorption injector.The temperature of Thermal desorption injector
Degree is at 180 DEG C.The sample gas that Thermal desorption obtains is by carrier gas (air, with injector resolution temperature 180 DEG C)
Bringing the ionized region of ion mobility spectrometry into, the flow of carrier gas is at 400sccm；Sample is ionized at ionized region
Positive and negative ion, by the ion gate periodically opened, enters the drift region being made up of uniform electric field,
Obtain in drift region separating and detection.See that Fig. 3 is ion mobility spectrometry detection saliva sample under positive ion mode
The ion migration spectrogram of product (containing KET 100ppm), the quasi-molecular ions at migration time 5.88ms and poison
The information of product storehouse KET matches.
Low concentration experimental verification, the method in the present invention can make detection sensitivity improve 1 order of magnitude.
The purpose adjusting pH value is to strengthen drugs dissolubility in saliva.Add assistant chemical additive purpose simultaneously
It is to promote the gasification of drugs Thermal desorption, and then improves detection sensitivity.
Claims (6)
1. the method for drugs in a quick detection saliva, it is characterised in that: with ion mobility spectrometry skill
Art is detection technique, adds aqueous slkali regulation pH value between 8.5-9.5 in saliva sample, then to tune
Saliva sample after joint pH adds assistant chemical additive, carries out with ion migration analysis of spectrum detector
Detection；The result of above-mentioned detection judges saliva with the contrast of drugs ion migration analysis of spectrum testing result spectrogram storehouse
Whether containing Poison in liquid.
Method the most according to claim 1, it is characterised in that: concrete analysis step is:
1) drugs standard substance analysis test: take drugs standard substance, with ion migration analysis of spectrum detector just
Carry out detection under ion mode to analyze, it is thus achieved that each Autonomous test signal；Determine drugs under positive ion mode
Go out peak migration time；Revise ion migration analysis of spectrum testing result spectrogram storehouse；
2) saliva sample analysis test: take saliva sample, first with the pH of aqueous slkali regulation saliva sample
It is worth between 8.5-9.5, is added to assistant chemical additive, detect with ion migration analysis of spectrum
Instrument carries out detection in the positive-ion mode and analyzes, it is thus achieved that each Autonomous test signal；The sample obtained according to it
Peak migration time and step 1) in the drugs signal peak migration time contrast of spectrogram storehouse, and then determine saliva
In whether containing Poison.
Method the most according to claim 1 and 2, it is characterised in that: concrete analysis step is:
1) drugs standard substance analysis test: one or two or more kinds drugs standard substance is dissolved in organic respectively
Solvent is made into the solution of 1-1000ppm；Above-mentioned solution carries out ion migration analysis of spectrum detection respectively, point
Huo get not detect signal, set up the detection of drugs standard substance ion migration analysis of spectrum with the detection signal obtained
Result spectrogram storehouse；Particularly as follows: take a kind of above-mentioned solution 10-100 μ L to drip to ion migration analysis of spectrum every time
At sampling corresponding on the sample introduction sheet of detector, then coupongs are sent into ion mobility spectrometry Thermal desorption sample introduction
In device, carrying out detection and analyze under ion mobility spectrometry positive ion mode, every kind of above-mentioned solution each obtains
Detection signal, determine drugs under positive ion mode goes out peak migration time；Revise ion migration analysis of spectrum
Testing result spectrogram storehouse；
2) saliva sample analysis test: accurately measure 100-500 μ L saliva sample, first molten with alkali
The pH value of liquid regulation saliva sample between 8.5-9.5, then sample introduction, measure above-mentioned saliva solution and exist
At the sample introduction sheet sampling of ion migration analysis of spectrum detector, saliva sample sampling volume is 10-50 μ L,
It is added to assistant chemical additive, then sample introduction sheet is sent into the pyrolysis of ion migration analysis of spectrum detector
In analysis injector；Under ion mobility spectrometry positive ion mode, carry out detection analyze, it is thus achieved that detection signal；
The sample peak migration time obtained according to it and step 1) in spectrogram storehouse drugs signal peak migration time pair
Ratio, if signal peak and step 1 in saliva sample) in spectrogram storehouse drugs signal peak migration time differ,
Then may determine that without the drugs in this spectrogram storehouse in this saliva sample, if signal peak and step in saliva sample
Rapid 1) the spectrogram storehouse drugs signal peak migration time in is identical, then need to detect further.
Method the most according to claim 3, it is characterised in that: regulate described in step (2)
The alkali liquor used during saliva sample pH is aqueous sodium carbonate or sodium bicarbonate aqueous solution, and concentration is
2·10-8.5Mol/L to 2 10-9.5Between mol/L.
Method the most according to claim 3, it is characterised in that: auxiliaryization described in step (2)
Learn additive be auxiliary Thermal desorption chemical addition agent methanol, ethanol or acetonitrile in one or two kinds or
Three kinds, the addition of assistant chemical additive is 1-10 times of described saliva sample sampling volume.
Method the most according to claim 3, it is characterised in that: described drug species can be suitable
Heal up clothes or suction drugs Opium, heroin, morphine, Fructus Cannabis, cocaine, head-shaking pill, methamphetamine hydrochloride,
Dolantin, KET, cherry chestnut, Opium, caffeine, amphetamines or methylene dioxygen methamphetamine
In one or more.
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| CN113740443A (en) * | 2020-05-29 | 2021-12-03 | 同方威视技术股份有限公司 | Detector for detecting drugs and metabolites thereof |
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