CN106198702B - 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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- CN106198702B CN106198702B CN201510226674.8A CN201510226674A CN106198702B CN 106198702 B CN106198702 B CN 106198702B CN 201510226674 A CN201510226674 A CN 201510226674A CN 106198702 B CN106198702 B CN 106198702B
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Abstract
The invention discloses a kind of methods of drugs in quickly detection saliva.It takes saliva sample that aqueous slkali is added and adjusts pH value, then measure above-mentioned saliva solution at sample introduction piece sampling, then add the assistant chemical additive of certain volume into saliva sample, sample introduction piece is sent into ion mobility spectrometry analysis detection instrument Thermal desorption sample injector.Output analysis detection result is detected through Thermal desorption post analysis.Measurement detection limit can achieve 1ng or less magnitude (0.1ppm or less concentration).Single sample analysis time is less than 5S, the automatic output test result of software.Measurement method simplicity, quick, efficient, good reliability in the present invention.Enter to take poison for mouth, drug abuse case, ion mobility spectrometry analysis detection instrument can realize quickly inspection by drug ingredient in detection saliva completely using the method in the present invention.Application study demand in terms of based on forensic science, software control instrument can implement alarm mode according to drugs transit time.
Description
Technical field
The invention discloses a kind of methods for quickly, sensitively detecting drugs in saliva, using Ion mobility spectrometry as base
This detection technique establishes the qualitative method that ion mobility spectrometry quickly detects drugs in saliva using positive and negative ion mode.
Background technique
In recent years, drugs are increasing to the harm of human lives, seriously threatened the normal life of the mankind.So
It is extremely important to the detection of drugs, especially consume illegal drugs the confirmation of people's crime fact.This measurement method is easy, quickly, efficiently,
Good reliability.Enter to take poison for mouth, drug abuse case, ion mobility spectrometry can be realized fast by drug ingredient in detection saliva completely
Fast screening.
Saliva is a kind of colourless and thin liquid, is commonly called as by people as saliva, although being referred to as in ancient times, " Jinin is beautiful
But always there are unclean indecency sense in liquid ", modern times to people.The liquid secreted by three pairs of major salivary glands (lower jaw gland, rib gland and sublingual gland)
The mucus of many small mucus glands secretes, the digestive juice mixed in oral cavity on body and oral cavity wall.Saliva colorless and odorless, PH are
6.6 to 7.1.The daily secretory volume of normal person is about 1.0 to 1.5 liters of (herbivores such as ox, sheep, daily salivary secretion amount up to bodies
The 1/3 of weight).99% is water in the saliva of people.
In recent years, by studying saliva, people have found that saliva has a variety of new purposes again.
Diagnose the illness: lesion occurs for body, and the chemical analysis of saliva is necessarily made also to change therewith.It only needs saliva
Drying generates crystallization, and crystal shape is different with lesion, thus may be used as diagnosing such as hypertension, parotitis, cholera, glycosuria
The evidence of disease, roundworm disease etc..
Diseases prevention anti-cancer: the ingredients such as mucoprotein in saliva can neutralize part gastric acid, generate precipitating, be attached on gastric mucosa,
Protective layer is formed, peptic ulcer can be prevented and treated.In addition, lysozyme contained in saliva, can not only kill or inhibit staphylococcus,
Typhoid bacillus, Escherichia coli, hemolytic streptococcus etc., but also the carcinogenic poison such as can make aflatoxins BaP, nitrosamine
Property substantially reduces, or even becomes innocuous substance.
Monitoring medication: after medication, saliva is acquired within a certain period of time, chemically examines its drug content, can know that the medicine exists
Concentration in blood.
The optimum utilization of saliva is to find disease.Saliva reflection is being studied now to lose with osteoporosis, hormone secretion
Reconcile artery sclerosis, the especially connection between the lethal illness such as AIDS.Expert points out that saliva is that detection drugs etc. are toxic
The active principle of substance.
The type of drugs is divided into according to abuse route: oral, suction or injection.Different drugs are also not to the injury of people
With, lethal mechanism is also different.Heroin is commonly called as " white powder ".It is a kind of drugs synthesized with morphine.It is right as morphine
Respiratory center has extremely strong inhibiting effect.And the effect of white powder is 5 times of morphine.It is too slow excessively to will cause heartbeat, expiratory dyspnea
And it is dead.Cocaine, the alkaloid extracted in coca leaf.Central nervous system has very toxic.Bone can be stimulated by excessively sucking
Marrow leads to respiratory failure and dead.Crystal methamphetamine and its derivative, are commonly called as ice, and primary raw material is ephedrine.Damage is big
Brain function, causes heart failure.Its derivative is novel amphetamine, that is, dancing outreach.Damage cardiovascular system and maincenter
Nervous system.Excessive use causes palpitating speed, and blood pressure rises and causes to set out internal haemorrhage and dead.In quick analysis detection saliva
Drugs are current very important problems.Ketamine (English: ketamine), is commonly called as Ketamine, Ketamine, Ketamine, ketamine, is one
The drugs of mental department (drugs) of kind danger close, belongs to department of anesthesia of non-opium system drug.Ketamine product is main seen in daily
Composition is ketalar, chemical formula C13H16ClNOHCl, molecular weight are 274.19.It is white under normal temperature and pressure
Powdered solid substance.Fusing point is 266 degree, noninflammability.PH value 3.5~5.5, aqueous solution is in acidity.
In recent years, drugs are increasing to the harm of human lives, and the number of drug abuse is increasing in the whole world, smuggling poison
The case where product, is increasingly severe, and illicit drugs inspection field is increasingly becoming important field.High performance liquid chromatography, immunoassay etc.
Chemical method is the traditional method of comparison.These methods have their respective limitations, such as compare detection environmental requirement
Height, detection cycle are long etc..Ion mobility spectrometry (Ion Mobility Spectrometry, IMS) 70 years 20th century of technology
A kind of separation detection technique that generation occurs has structure simple compared with traditional mass spectrum, chromatographic apparatus, high sensitivity, analysis
Speed is fast, as a result reliable feature.Micro substance can be detected in atmospheric environment, be suitable for scene and use.It therefore can
By the on-line checking of the technical application to precursor chemicals.
Summary of the invention
The object of the present invention is to provide a kind of methods that drugs in saliva are quickly detected using ion mobility spectrometry.In order to realize
Direct, quick, the sensitive detection of drugs, the technical solution adopted by the present invention in saliva are as follows:
1) drugs Standard analysis tests: taking 10-100 μ L drugs standard items to drip at the corresponding sampling of sample introduction on piece, then will
Coupongs are sent into ion mobility spectrometry Thermal desorption sample injector.It is tested and analyzed under ion mobility spectrometry positive ion mode respectively,
Obtain each autonomous test signal；Determine the appearance transit time of drugs under positive ion mode；
2) saliva sample analysis test: it is accurate to measure 100-500 μ L saliva sample, first addition aqueous slkali (sodium carbonate or
Sodium bicarbonate) it adjusts between pH value 8.5-9.5, the above-mentioned saliva solution of 10-50 μ L is then measured at sample introduction piece sampling, while to
The assistant chemical additive of 1-10 times of volume is added in saliva sample, then sample introduction piece is sent into ion mobility spectrometry analysis detection instrument heat
It parses in sample injector.It is tested and analyzed under ion mobility spectrometry positive ion mode respectively, obtains each autonomous test signal；According to it
It is in the sample peak transit time of acquisition and the spectrogram library drugs signal peak transit time comparison in step 1) and then determining saliva
It is no to contain Poison.
The aqueous slkali of above-mentioned addition certain volume is adjusted in pH value method, and the lye volume of addition is equal to taking for saliva sample
Sample volume, lye refer to sodium carbonate or sodium bicarbonate aqueous solution.
Sodium carbonate or sodium bicarbonate aqueous solution concentration are 2 × 10-8.5Mol/L to 2 × 10-9.5Between mol/L.
In the analysis of sample introduction piece sample detection, while auxiliary Thermal desorption chemical addition agent methanol, ethyl alcohol or acetonitrile are added, it can
To greatly improve detection sensitivity.
Thermal desorption chemical addition agent is assisted, auxiliary Thermal desorption chemical addition agent is mixed with saliva sample, describedization
Additive is anhydrous reagent, and additive amount is 1-10 times of saliva sample sampling volume.
Method in the present invention can detect respectively be suitble to oral or suction drugs opium, heroin, morphine, hemp,
Cocaine, head-shaking pill, methamphetamine, Sauteralgyl, Ketamine, cherry chestnut, opium, caffeine, amphetamine, methylene dioxygen methamphetamine
Advantages of the present invention is as follows:
1. live quickly analysis in situ, online may be implemented as drugs analysis means in saliva in ion mobility spectrometry.
2. entire instrument total amount is less than 10kg, equipment instrument is small and exquisite portable, easy to carry, instrument independent operating, is suitble to existing
Field uses；
3. measuring speed is fast；Not complicated sample pre-treatments test, is very suitable to on-site quick screening；The operation of instrument
Expense is very low, and consumables are seldom；The cost performance of instrument is high, analyzes alarm velocity in 5 seconds.
4. measurement method adjusts saliva PH value and assistant chemical additive can greatly improve detection sensitivity: the present invention
In method can make detection sensitivity improve 1 order of magnitude；The purpose for adjusting pH value is the solubility for increasing drugs in saliva.
Add the purpose of assistant chemical additive simultaneously is to promote the gasification of drugs Thermal desorption, and then improve detection sensitivity.
Detailed description of the invention
Fig. 1 is the ion mobility spectrometry apparatus principle schematic diagram for detecting drugs in saliva；
1 is ionized region, and 2 be migration area, and 3 be Thermal desorption sample injector, and 4 be gas-carrier pipeline, and 5 be ion source, and 6 be gas outlet, 7
For ion gate, 8 is migrate ring in migration tube, 9 be aperture plate, and 10 be drift air pipe, and 11 be detector；
Fig. 2 is ion mobility spectrometry background signal ion transfer spectrogram (RIP) under positive ion mode；
Fig. 3 is the ion transfer spectrogram that ionic migration spectrum detection Ketamine content is 100ppm saliva sample under positive ion mode；
Specific embodiment
In following embodiment the operation of involved ion mobility spectrometry using the ion mobility spectrometry apparatus of structure shown in Fig. 1 into
Row detection；The experiment condition of following embodiment intermediate ion migration spectrum is equal are as follows: ionization source is radioactivity63The ion mobility spectrometry in the source Ni,
Stepper motor sample injector.Migration tube temperature is maintained at 100 DEG C when experiment, and 180 DEG C of sample injector temperature, carrier gas (air), drift gas are (empty
Gas) air-flow is respectively 400,600mL/min.Saliva sample containing drugs is after Thermal desorption heating devices heat, and drugs are with auxiliary
Additive volatilizees together, and sample introduction is analyzed detects.
It, will be every in order to realize that quick, the Sensitive Detection of drugs in saliva, the present invention use ion mobility spectrometry as analysis means
Kind drugs standard items are dissolved in organic solvent (solution for being made into 1-1000ppm) respectively, as calibrating reagent sample, drip to respectively
Sample introduction on piece obtains detection signal, in detector software in the positive-ion mode using ionic migration spectrometer as detecting instrument respectively
The transit time information of the different drugs of input, establishes drugs standard items ion mobility spectrometry analysis detection result spectrogram library in system,
Software identifies detection of the mobility information for drugs in sample to be tested.
Embodiment 1
Air background detection:
The blank sampling sheet of no any sample of addition is sent into ion mobility spectrometry analysis detection instrument Thermal desorption sample injector.
The temperature of Thermal desorption sample injector is at 180 DEG C.The sample gas that Thermal desorption obtains is by carrier gas (air, with sample injector resolution temperature 180
DEG C) bring the ionized region of ion mobility spectrometry into, the flow of carrier gas is in 400sccm；Sample is ionized to positive and negative ion in ionized region,
Separation is obtained in drift region and is obtained with detection into the drift region being made of uniform electric field by the ion gate periodically opened
Instrumental background detects signal.Fig. 2 gives the ion transfer spectrogram with positive ion mode ionic migration spectrum detection air background, from
In figure as can be seen that positive ion mode reagent ion peak (RIP) occurs about in 4.36ms.
Embodiment 2
Saliva background detection:
It is as follows using the process of ionic migration spectrum detection blank saliva sample using method provided by the invention: to take saliva sample
Sodium bicarbonate aqueous solution (2 × 10 is added in product-9Mol/L pH value) is adjusted 9, then measures the 50 above-mentioned saliva solutions of μ L in sample introduction
At piece sampling, while isometric assistant chemical additive ethyl alcohol is added into saliva sample, then sample introduction piece feeding ion is moved
It moves in spectrum analysis detector Thermal desorption sample injector.The temperature of Thermal desorption sample injector is at 180 DEG C.The sample gas quilt that Thermal desorption obtains
The ionized region of ion mobility spectrometry is brought in carrier gas (air, with sample injector resolution temperature 180 DEG C) into, and the flow of carrier gas is in 400sccm；Sample
Product are ionized to positive and negative ion in ionized region, by the ion gate periodically opened, into the drift being made of uniform electric field
Area obtains separation and detection in drift region.Saliva detection signal also only has air reagent ion peak (RIP) to go out under positive ion mode
Present 4.36ms or so, saliva background is interfered without other signals.
Embodiment 3
The detection of drugs in saliva sample:
Process using ketamine (Ketamine) in ionic migration spectrum detection saliva is as follows:
(1) drugs Standard analysis tests: by ketamine (Ketamine), opium is dissolved in respectively 95% alcohol solvent, is made into respectively
The solution of 100-500ppm；Two kinds of solution carry out ion mobility spectrometry analysis detection respectively, detection signal are obtained respectively, with acquisition
Detection signal establishes drugs standard items ion mobility spectrometry analysis detection result spectrogram library；Specifically: take above-mentioned 1 μ L drop of Ketamine solution
To at the corresponding sampling of sample introduction on piece of ion mobility spectrometry analysis detection instrument, then by coupongs be sent into ion mobility spectrometry Thermal desorption into
In sample device, tested and analyzed under ion mobility spectrometry positive ion mode；Above-mentioned opium solution is taken to repeat above operation, two kinds molten
Liquid respectively obtains detection signal, determines the appearance transit time of drugs under positive ion mode；Correct ion mobility spectrometry analysis detection
As a result spectrogram library, wherein the transit time of Ketamine is 5.88ms, the transit time 9.36ms of opium.The above Ion transfer spectrum analysis
Condition is equal are as follows: the temperature of Thermal desorption sample injector is at 180 DEG C.The sample gas that Thermal desorption obtains is by carrier gas (air, with sample injector solution
180 DEG C of eutectoid temperature) bring the ionized region of ion mobility spectrometry into, the flow of carrier gas is in 400sccm.
(2) saliva sample analysis test: saliva sample (containing Ketamine 100ppm) is taken, sodium bicarbonate aqueous solution (2 × 10 is added- 9Mol/L it) adjusts pH value and then measures the 50 above-mentioned saliva solutions of μ L at sample introduction piece sampling 9, while adding into saliva sample
Add isometric assistant chemical additive ethyl alcohol, then sample introduction piece is sent into ion mobility spectrometry analysis detection instrument Thermal desorption sample injector
It is interior.The temperature of Thermal desorption sample injector is at 180 DEG C.The sample gas that Thermal desorption obtains is by carrier gas (air, with sample injector resolution temperature
180 DEG C) bring the ionized region of ion mobility spectrometry into, the flow of carrier gas is in 400sccm；Sample ionized region be ionized to it is positive and negative from
Son, into the drift region being made of uniform electric field, obtains separation and detection in drift region by the ion gate periodically opened.
See that Fig. 3 is the ion transfer spectrogram of ionic migration spectrum detection saliva sample under positive ion mode (containing Ketamine 100ppm), in migration
Between quasi-molecular ions at 5.88ms match with the information of drug library Ketamine.
Low concentration experimental verification, the present invention in method can make detection sensitivity improve 1 order of magnitude.Adjust the mesh of pH value
Be to increase solubility of the drugs in saliva.Adding the purpose of assistant chemical additive simultaneously is to promote the gasification of drugs Thermal desorption, into
And improve detection sensitivity.
Claims (6)
1. a kind of method of drugs in quickly detection saliva, it is characterised in that: using Ion mobility spectrometry as detection technique, saliva
Aqueous slkali is added in sample and adjusts pH value between 8.5-9.5, then adds to addition assistant chemical in the saliva sample after pH is adjusted
Add agent, is detected with ion mobility spectrometry analysis detection instrument；The result and drugs ion mobility spectrometry analysis detection knot of above-mentioned detection
The comparison of fruit spectrogram library determines whether contain Poison in saliva；
The assistant chemical additive added in saliva sample is one of methanol, ethyl alcohol or acetonitrile or two kinds or three
Kind.
2. according to the method described in claim 1, it is characterized by: concrete analysis step are as follows:
1) drugs standard items analysis test: drugs standard items are taken, are carried out under ion mobility spectrometry analysis detection instrument positive ion mode
It tests and analyzes, obtains each autonomous test signal；Determine the appearance transit time of drugs under positive ion mode；Correct ion mobility spectrometry point
Analyse testing result spectrogram library；
2) saliva sample analysis test: taking saliva sample, adjusted first with aqueous slkali the pH value of saliva sample to 8.5-9.5 it
Between, assistant chemical additive is added thereto, is tested and analyzed in the positive-ion mode with ion mobility spectrometry analysis detection instrument,
Obtain each autonomous test signal；When the spectrogram library drugs signal peak in sample peak transit time and step 1) obtained according to it migrates
Between compare, and then determine saliva in whether contain Poison.
3. method according to claim 1 or 2, it is characterised in that: concrete analysis step are as follows:
1) drugs standard items analysis test: one or two or more kinds of drugs standard items are dissolved in organic solvent respectively and are made into 1-
The solution of 1000ppm；Above-mentioned solution carries out ion mobility spectrometry analysis detection respectively, detection signal is obtained respectively, with the inspection of acquisition
It surveys signal and establishes drugs standard items ion mobility spectrometry analysis detection result spectrogram library；Specifically: a kind of above-mentioned solution 10- is taken every time
100 μ L are dripped at the corresponding sampling of sample introduction on piece of ion mobility spectrometry analysis detection instrument, then coupongs are sent into ion mobility spectrometry
It in Thermal desorption sample injector, is tested and analyzed under ion mobility spectrometry positive ion mode, every kind of above-mentioned solution is respectively detected
Signal determines the appearance transit time of drugs under positive ion mode；Correct ion mobility spectrometry analysis detection result spectrogram library；
2) saliva sample analysis test: it is accurate to measure 100-500 μ L saliva sample, the pH of saliva sample is adjusted with aqueous slkali first
Value is between 8.5-9.5, and then sample introduction, the sample introduction piece for measuring above-mentioned saliva solution in ion mobility spectrometry analysis detection instrument sample
Place, saliva sample sampling volume are 10-50 μ L, add assistant chemical additive thereto, then sample introduction piece is sent into Ion transfer
In spectrum analysis detector Thermal desorption sample injector；It is tested and analyzed under ion mobility spectrometry positive ion mode, obtains detection signal；
The spectrogram library drugs signal peak transit time in sample peak transit time and step 1) obtained according to it compares, if saliva sample
Middle signal peak and the spectrogram library drugs signal peak transit time in step 1) be not identical, then can determine that nothing should in the saliva sample
Drugs in spectrogram library, if signal peak is identical as the spectrogram library drugs signal peak transit time in step 1) in saliva sample,
It need to further be detected.
4. according to the method described in claim 3, the alkali used when it is characterized by: adjusting saliva sample pH described in step 2)
Solution is aqueous sodium carbonate or sodium bicarbonate aqueous solution, concentration 210-8.5Mol/L to 210-9.5Between mol/L.
5. according to the method described in claim 3, it is characterized by: the additive amount of assistant chemical additive described in step 2) is
1-10 times of the saliva sample sampling volume.
6. according to the method described in claim 3, it is characterized by: the drug species are to be suitble to oral or suction drugs crow
Piece, heroin, hemp, cocaine, head-shaking pill, methamphetamine, Sauteralgyl, Ketamine, caffeine, amphetamine or methylene dioxygen methyl peace
It is non-he hit it is one or more.
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| CN107219295A (en) * | 2017-05-15 | 2017-09-29 | 上海电机学院 | A kind of methamphetamine detection method based on ion mobility spectrometry |
| CN107356659A (en) * | 2017-07-03 | 2017-11-17 | 宁波华仪宁创智能科技有限公司 | The system and method taken drugs by saliva detection |
| CN107561150A (en) * | 2017-07-03 | 2018-01-09 | 宁波华仪宁创智能科技有限公司 | The detection method of drug abuse |
| CN109507355B (en) * | 2019-01-17 | 2021-02-02 | 浙江工业大学 | Method for determining content of syphilis and ecstasy in human hair by flash evaporation-gas chromatography-mass spectrometry |
| CN110823831A (en) * | 2019-11-18 | 2020-02-21 | 上海应用技术大学 | Far infrared detection method for drugs |
| CN111276385B (en) * | 2020-02-13 | 2020-12-08 | 清华大学 | Ion excitation detection method of mass spectrometer |
| 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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