CN110286187A - The detection method of human poisoning product - Google Patents
The detection method of human poisoning product Download PDFInfo
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- CN110286187A CN110286187A CN201810226040.6A CN201810226040A CN110286187A CN 110286187 A CN110286187 A CN 110286187A CN 201810226040 A CN201810226040 A CN 201810226040A CN 110286187 A CN110286187 A CN 110286187A
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Abstract
The present invention provides a kind of detection method of human poisoning product, comprising the following steps: a series of mixing drugs standard solution of gradient concentrations is prepared using 14 kinds of drugs standard items；Using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS), sample and the mixing drugs standard solution are subjected to Mass Spectrometer Method respectively, based on Mass Spectrometer Method as a result, determining that there are one of described mixing drugs standard solution or a variety of drugs in the sample, to realize qualitative analysis；Draw standard curve, and the peak area of the corresponding parent ion/daughter ion pair of at least one of described 14 kinds of drugs in the detection sample, and the concentration of the sample is obtained according to the standard curve, with quantitative analysis, optionally, the sample source is in people's saliva, and optionally, the sample is by pretreatment.The present invention has many advantages, such as that materials are convenient, dosage is few, detection limit and quantitative limit are low, accuracy is high and efficient.
Description
Technical field
The present invention relates to a kind of biological medicine detection technique fields, and in particular to a kind of detection method of human poisoning product.
Background technique
Drugs are increasing to the harm of human lives, and drug smuggling and drug abuse are just becoming a rapid development and day
The serious social concern of benefit.The drugs that drug addict sucks mainly include heroin, morphine, methamphetamine, ketamine, hemp and shake the head
Ball etc. brings serious harm to the life of oneself and surrounding population in view of consuming illegal drugs, therefore is badly in need of establishing a kind of internal
The detection method of drugs accurately rapidly and efficiently.
Saliva is mixed by the mucus of small mucus glands secretes many on sublingual gland, lower jaw gland, rib gland and oral cavity wall
Digestive juice.In recent years, pass through the research to saliva, it has been found that saliva has a variety of new purposes.Drugs enter quilt after human body
It absorbs, and is further metabolized quickly, free state drug can be turned by Passive diffusion, active transport and ultrafiltration cross-film in blood
It is transported to saliva.Saliva can partially substitute blood, urine and hair and studied and detected in terms of drug abuse.Relatively
For other body fluid samples, the collection of saliva is not limited by place, time, is easily received by subject, collection process is not invaded
Violate personal privacy, sampling process is easy to monitor, can be to avoid the imitation behavior of sample.In police law execution practice, saliva is utilized
Liquid has become a kind of common, easy detection method as sample.
Domestic and international drug abuse and its common analysis method of metabolin include enzyme immunoassay (EIA), radio-immunity
Measuring method (RIA), gas chromatography (GC), gas chromatography-mass spectrometry (GC-MS), high performance liquid chromatography (HPLC), liquid
Phase chromatograph-mass spectrometer coupling method (LC-MS) etc..Currently, inspection and quarantine department carries out the side of illicit drugs inspection to inward and outward personnel's urine
Method mainly uses colloidal gold technique, and false positive rate is high.It is the prior art for detecting material with saliva, basic principle is based on enzyme
Linked immunosorbent assay.And illicit drugs inspection kit majority is the detection kit of unitem or same class drugs, and type is less.And
And have the shortcomings that accuracy is lower, false positive is high in terms of testing result.
Summary of the invention
In view of the foregoing, it is necessary to which a kind of detection method of high, efficient human poisoning product of accuracy is provided.
The detection method of the human poisoning product, comprising the following steps:
A series of mixing drugs standard solution of gradient concentrations is prepared using 14 kinds of drugs standard items；
Using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS), by sample and the mixing drugs standard solution respectively into
Row Mass Spectrometer Method based on Mass Spectrometer Method as a result, when having the following conditions at the same time, determines that there are the admixture poisons in the sample
One of product standard solution or a variety of drugs, to realize qualitative analysis: (1) in the mass spectrogram of the sample and the mixing
There is the corresponding parent ion/daughter ion of at least one of identical 14 kinds of drugs in the mass spectrogram of drugs standard solution
It is right；(2) the chromatographic peak retention time of each pair of parent ion/daughter ion pair present in the sample with described to mix drugs standard molten
The corresponding chromatographic peak retention time relative error of liquid is less than 2%；(3) each pair of parent ion/daughter ion pair existing for the sample
Relative abundance than with the relative abundance of the corresponding parent ion/daughter ion pair of the mixing drugs standard solution than consistent；
Draw standard curve, and parent ion/daughter ion pair peak face of the drugs present in the detection sample
Product, and the concentration of the sample is obtained according to the standard curve, with quantitative analysis.
Optionally, the sample source is in people's saliva.
Optionally, the sample is by pretreatment.
Further, it is reversed that the determination condition of the Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS), which includes: liquid phase column,
Chromatographic column；Column temperature is 40 DEG C~55 DEG C；Mobile phase includes mobile phase A and Mobile phase B, and the mobile phase A is 2~10mmol/L's
Ammonium formate solution, the Mobile phase B are formic acid-acetonitrile solution, the volume of the ammonium formate solution and the formic acid-acetonitrile solution
Than for 1:15~15:1；Flow velocity is 400 μ of μ L/min~600 L/min.
Further, the pretreatment includes: to be centrifuged after mixing the saliva, takes supernatant, deionized water, whirlpool is added
Rotation concussion, is added precipitating reagent, is vortexed again for shaking, be centrifuged and taking supernatant.
Further, the precipitating reagent is selected from sulfosalisylic acid solution, urea or guanidine hydrochloride.
Further, the volume ratio of the saliva, the deionized water and the precipitating reagent is 1:1:1-1:2:3.
It further, include amphetamine, methylbenzene third with the drugs that the detection method of the human poisoning product detects
Amine, 3,4- methylene benzylene chloride propylamine, ketamine, heroin, morphine, codeine, pethidine, methadone, fentanyl,
One of 6- monoacetylmorphine, tetrahydrocannabinol, benzoyl ecgonine, cocaine are a variety of.
Further, it is electric that the determination condition of the Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS), which further includes ion source,
Spraying ionization-positive ion mode (ESI+)；Detection mode is multiple-reaction monitoring (MRM)；The pressure of gas curtain gas is 10-55Psi；It touches
Hitting atmospheric pressure is 0-12Psi；Atomization temperature is 0-550 DEG C；Atomization gas pressure is 0-90Psi.
Further, in carrying out the qualitative analysis, the corresponding parent ion/son of each drugs in 14 kinds of drugs
Ion pair is all made of two pairs, wherein two pairs of parent ion/daughter ions of every kind of drugs are to being respectively as follows: the amphetamine: 136.1/
91.1,136.1/119.1, the crystal methamphetamine: 150.2/91.1,150.2/119.1,3, the 4- methylene dioxy first
Base amphetamine: 194.1/163.1,194.1/105.2, the ketamine: 238.1/125.2,238.1/220.1, the Hai Luo
Cause: 370.2/328.2,370.2/268.2, the morphine: 286.1/165.0,286.1/201.0, the codeine:
300.1/165.1,300.1/215.1, the pethidine: 248.1/174.1,248.1/220.1, the methadone: 310.2/
265.2,310.2/265.2, the fentanyl: 337.2/188.1,337.2/105.1, the 6- monoacetylmorphine: 328.1/
211.3,328.1/165.3, the tetrahydrocannabinol: 315.2/259.2,315.2/193.2, the benzoyl ecgonine:
290.1/168.1,290.1/105.2, the cocaine: 304.1/182.1,304.1/150.2.
Further, in carrying out the quantitative analysis, for the drugs present in the sample, two couples of mothers are selected
Ion/daughter ion at least one of detection peak area, wherein two pairs of parent ion/daughter ions of every kind of drugs are to being respectively as follows:
State amphetamine: 136.1/91.1,136.1/119.1, the crystal methamphetamine: 150.2/91.1,150.2/119.1, described 3,
4- methylene benzylene chloride propylamine: 194.1/163.1,194.1/105.2, the ketamine: 238.1/125.2,
238.1/220.1, the heroin: 370.2/328.2,370.2/268.2, the morphine: 286.1/165.0,286.1/
201.0, the codeine: 300.1/165.1,300.1/215.1, the pethidine: 248.1/174.1,248.1/220.1,
The methadone: 310.2/265.2,310.2/265.2, the fentanyl: 337.2/188.1,337.2/105.1, the 6-
Monoacetylmorphine: 328.1/211.3,328.1/165.3, the tetrahydrocannabinol: 315.2/259.2,315.2/193.2, institute
State benzoyl ecgonine: 290.1/168.1,290.1/105.2, the cocaine: 304.1/182.1,304.1/150.2.
Further, carried out in the quantitative determination in the drugs, the range of detection limit 0.02ng/mL extremely
Between 0.14ng/mL, the range of quantitative limit is in 0.1ng/mL between 0.5ng/mL.
The present invention utilizes Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS), by the mixing for configuring 14 kinds of drugs standard items
Standard solution qualitatively or quantitatively can detect one of this 14 kinds of drugs or a variety of simultaneously, easy to operate, detection limit and
Quantitative limit is low, accuracy is high and it is efficient the advantages that, and saliva is selected to be detected, compared with prior art, draw materials it is convenient, use
Amount is few.
Detailed description of the invention
For the above objects, features and advantages of the present invention can more be become apparent, below in conjunction with attached drawing to tool of the invention
Body embodiment elaborates, in which:
Fig. 1 is the MRM map of the mixing sample for being used to simulate authentic specimen of the offer of the embodiment of the present invention 1.
Fig. 2 is the canonical plotting for the amphetamine that the embodiment of the present invention 1 provides.
Fig. 3 is the canonical plotting for the crystal methamphetamine that the embodiment of the present invention 1 provides.
Fig. 4 is the canonical plotting for the 3,4- methylenedioxymethamphetamine (MDMA) that the embodiment of the present invention 1 provides.
Fig. 5 is the canonical plotting for the ketamine that the embodiment of the present invention 1 provides.
Fig. 6 is the canonical plotting for the heroin that the embodiment of the present invention 1 provides.
Fig. 7 is the canonical plotting for the morphine that the embodiment of the present invention 1 provides.
Fig. 8 is the canonical plotting for the codeine that the embodiment of the present invention 1 provides.
Fig. 9 is the canonical plotting for the pethidine that the embodiment of the present invention 1 provides.
Figure 10 is the canonical plotting for the methadone that the embodiment of the present invention 1 provides.
Figure 11 is the canonical plotting for the fentanyl that the embodiment of the present invention 1 provides.
Figure 12 is the canonical plotting for the monoacetylmorphine that the embodiment of the present invention 1 provides.
Figure 13 is the canonical plotting for the tetrahydrocannabinol (THC) that the embodiment of the present invention 1 provides.
Figure 14 is the canonical plotting for the benzoyl ecgonine that the embodiment of the present invention 1 provides.
Figure 15 is the canonical plotting for the cocaine that the embodiment of the present invention 1 provides.
Figure 16 is that the embodiment of the present invention 2 provides the mixing sample MRM map for being used to simulate authentic specimen.
Figure 17 is the canonical plotting for the heroin that the embodiment of the present invention 2 provides.
Figure 18 is the MRM map for the authentic specimen that the embodiment of the present invention 3 provides.
Figure 19 is the canonical plotting for the ketamine that the embodiment of the present invention 3 provides.
Specific embodiment
In order to be illustrated concise and clearly, in appropriate place, identical label is repeatedly used in different drawings
In the corresponding or similar element of mark.In addition, in order to provide to embodiment described herein deep understanding comprehensively, explanation
Many specific details can be referred in book.However, it will be understood by those skilled in the art that embodiment recited herein
It can not be operated according to these specific details.In other cases, in order not to keeping the technology being described special
Levy confused, certain methods, process and element are not described in detail.It is not absolutely required to the sizes etc. with material object for schema
Together.In order to which details and technical characteristic is better described, the displaying ratio of specific part may be amplified in schema.In specification
Description be not considered as the restriction to scope of embodiments described herein.
The embodiment of the present invention provides a kind of detection method of human poisoning product, comprising the following steps:
Step 1: a series of mixing drugs standard solution of gradient concentrations is prepared using 14 kinds of drugs standard items；
Step 2: using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS), by the sample and the mixing drugs standard
Solution carries out Mass Spectrometer Method respectively, based on Mass Spectrometer Method as a result, when having the following conditions at the same time, determines and exists in the sample
One of described mixing drugs standard solution or a variety of drugs, to realize qualitative analysis: (1) in the mass spectrogram of the sample
With exist in the mass spectrogram of the mixing drugs standard solution at least one of identical described 14 kinds of drugs it is corresponding it is female from
Son/daughter ion pair；(2) the chromatographic peak retention time of each pair of parent ion/daughter ion pair present in the sample is mixed with described
The corresponding chromatographic peak retention time relative error of drugs standard solution is less than 2%；(3) existing for the sample it is each pair of it is female from
Relative abundance of son/daughter ion pair relative abundance than parent ion/daughter ion pair corresponding with the mixing drugs standard solution
Than consistent；
Step 3: drawing standard curve, and parent ion/daughter ion pair of the drugs present in the detection sample
Peak area, and the concentration of the sample is obtained according to the standard curve, with quantitative analysis.
Wherein, it should be noted that expression way " each pair of parent ion/son existing for the sample used by herein
The relative abundance of ion pair than with the relative abundance of the corresponding parent ion/daughter ion pair of the mixing drugs standard solution than one
Cause " refer to: the relative abundance ratio of each pair of parent ion/daughter ion pair existing for the sample and the mixing drugs standard solution pair
Parent ion/daughter ion pair the relative abundance answered is no more than range listed by table 1 than identical or relative error.
Table 1: the maximum allowable relative error (%) of relative abundance ratio
Optionally, the sample source is in people's saliva.The saliva that the present invention is flowed out naturally using people is as sample, and materials are just
Victory, dosage are few.
Optionally, the sample is by pretreatment.Further, sample pretreatment includes being centrifuged after mixing saliva, is taken
Deionized water is added in supernatant, and be vortexed concussion, and precipitating reagent is added, be vortexed again for shaking, be centrifuged and take supernatant to get to
Test sample.
Wherein, the precipitating reagent is selected from sulfosalisylic acid solution, urea or guanidine hydrochloride, and the precipitating reagent is mainly used to precipitate
Protein and some heavy metal ion in saliva.In the present embodiment, the precipitating reagent is sulfosalisylic acid solution, the sulphur
Base salicylic acid with good water solubility, stabilization, it is nontoxic, there is the excellent of stronger binding ability to transition metal and heavy metal ion
Point.
Further, the volume ratio range of saliva, deionized water and precipitating reagent is 1:1:1~1:2:3.In the present embodiment
In, the mass concentration range of the sulfosalicylic acid is 1%~10%.
In step 1, the present invention is using the mixing drugs standard solution for containing 14 kinds of drugs standard items.14 kinds of poison
Product include amphetamine, crystal methamphetamine, 3,4- methylene benzylene chloride propylamine, ketamine, heroin, morphine, codeine,
Pethidine, methadone, fentanyl, 6- monoacetylmorphine, tetrahydrocannabinol, benzoyl ecgonine, in cocaine.Really detecting
In the process, when standard items configure, do not know which kind of drugs sample to be tested contains, it, can be when detection is one of or several drugs
Testing result eliminates other data other than object when calculating, easy to operate, error is small.It should be understood that described in
The drugs of the detection method detection of human poisoning product include amphetamine, crystal methamphetamine, 3,4- methylene dioxy methyl
Amphetamine, ketamine, heroin, morphine, codeine, pethidine, methadone, fentanyl, 6- monoacetylmorphine, tetrahydro hemp
One of phenol, benzoyl ecgonine, cocaine are a variety of.
Further, 14 kinds of drugs standard items substances are taken respectively, are diluted step by step with deionized water, it is dense to configure a series of gradients
The standard solution of degree.The concentration of the standard solution of the series, for example, 0.1ng/mL, 0.5ng/mL, 1.0ng/mL, 10ng/mL,
Then 50ng/mL, 100ng/mL respectively mix the standard solution of the respective concentration of 14 kinds of drugs, spare.
In step 2, it is anti-that the testing conditions of the Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS), which include: liquid phase column,
To chromatographic column；Column temperature is 40 DEG C~55 DEG C；Mobile phase includes mobile phase A and Mobile phase B, and the mobile phase A is 2~10mmol/L
Ammonium formate solution, the Mobile phase B be formic acid-acetonitrile solution, the body of the ammonium formate solution and the formic acid-acetonitrile solution
Product is than being 1:15~15:1；Flow velocity is 400 μ of μ L/min~600 L/min.
The determination condition of the Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) further comprises: ion source is electron spray
Ionization-positive ion mode (ESI+)；Detection mode is multiple-reaction monitoring (MRM)；The pressure of gas curtain gas is 10-55Psi；Collision gas
Pressure is 0-12Psi；Atomization temperature is 0-550 DEG C；Atomization gas pressure is 0-90Psi.
Further, the reverse chromatograms column is selected from 50 × 2.1mm of ACE.EXCEL2C18, ACQUITY UPLC HSS
T3.100 × 2.1mm or the comparable chromatographic column of other performances.
In the present embodiment, the analysis parameter such as table 2 of the Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) of 14 kinds of drugs:
The LC-MS/MS of table 2:14 kind drugs analyzes parameter
Note: * is quota ion pair
In table 2, the DP is to remove cluster voltage, and the CE is collision energy, and RT is retention time.It is to be appreciated that sample
Product be when entering mass spectrum it is tufted, similar to the state of droplet, go cluster voltage DP for smashing tufted sample.
Collision energy CE is that parent ion is broken into daughter ion.During atual detection, instrument parameter setting the inside can be set
The detection parameters of 14 kinds of drugs, the various time points that measuring samples enter instrument detection are to repeat to detect 14 kinds by the parameter of setting
Object.
Specifically, after sample introduction, if the corresponding chromatography of the chromatographic peak retention time of sample and mixing drugs standard solution
Peak retention time compares, and relative error occurs selected less than 2%, and in the sample mass spectrum after background correction
Ion pair, and selected ion pair relative abundance is no more than than the relative error of the ion pair relative abundance ratio with reference substance
Defined range then can determine whether that there are one of described mixing drugs standard solution or a variety of drugs in sample.It is understood that
, for same substance under the conditions of identical Mass Spectrometer Method, ratio i.e. the relative abundance ratio of parent ion and daughter ion are one
It is fixed, when relative abundance than with the relative abundance of mixing drugs standard solution than consistent, both it can be assumed that for same substance, as
Qualitative detection.
In the present invention, in carrying out the qualitative analysis, the corresponding parent ion of each drugs in 14 kinds of drugs/
Daughter ion is to being all made of two pairs, wherein two pairs of parent ion/daughter ions of every kind of drugs are to being respectively as follows: the amphetamine: 136.1/
91.1,136.1/119.1, the crystal methamphetamine: 150.2/91.1,150.2/119.1,3, the 4- methylene dioxy first
Base amphetamine: 194.1/163.1,194.1/105.2, the ketamine: 238.1/125.2,238.1/220.1, the Hai Luo
Cause: 370.2/328.2,370.2/268.2, the morphine: 286.1/165.0,286.1/201.0, the codeine:
300.1/165.1,300.1/215.1, the pethidine: 248.1/174.1,248.1/220.1, the methadone: 310.2/
265.2,310.2/265.2, the fentanyl: 337.2/188.1,337.2/105.1, the 6- monoacetylmorphine: 328.1/
211.3,328.1/165.3, the tetrahydrocannabinol: 315.2/259.2,315.2/193.2, the benzoyl ecgonine:
290.1/168.1,290.1/105.2, the cocaine: 304.1/182.1,304.1/150.2.As shown in Table 1, it is possible to understand that
, two pairs of parent ion/daughter ion pair retention times of every kind of drugs are the same.
In step 3, the embodiment of the present invention is quantified using external standard method.It should be understood that the drugs in sample to be tested
Concentration should the range of linearity in.With first parent ion/daughter ion of object to peak area (Y) for ordinate, target
Amount of substance concentration (C) is that abscissa draws standard curve, is quantified with standard curve to sample.
In the present embodiment, in carrying out the quantitative analysis, for the drugs present in the sample, two are selected
To parent ion/daughter ion at least one of detection peak area, wherein two pairs of parent ion/daughter ions of every kind of drugs to respectively
Are as follows: the amphetamine: 136.1/91.1,136.1/119.1, the crystal methamphetamine: 150.2/91.1,150.2/119.1,
3, the 4- methylene benzylene chloride propylamine: 194.1/163.1,194.1/105.2, the ketamine: 238.1/125.2,
238.1/220.1, the heroin: 370.2/328.2,370.2/268.2, the morphine: 286.1/165.0,286.1/
201.0, the codeine: 300.1/165.1,300.1/215.1, the pethidine: 248.1/174.1,248.1/220.1,
The methadone: 310.2/265.2,310.2/265.2, the fentanyl: 337.2/188.1,337.2/105.1, the 6-
Monoacetylmorphine: 328.1/211.3,328.1/165.3, the tetrahydrocannabinol: 315.2/259.2,315.2/193.2, institute
State benzoyl ecgonine: 290.1/168.1,290.1/105.2, the cocaine: 304.1/182.1,304.1/150.2.
In embodiments of the present invention, the detection method of the human poisoning product can carry out qualitative and quantitative point simultaneously
Analysis, in other embodiments, the detection method of human poisoning product can also individually carry out qualitative analysis or quantitative analysis.
In embodiments of the present invention, in the quantitative analysis, the range of the detection limit of the drugs 0.02ng/mL extremely
Between 0.14ng/mL, the range of the quantitative limit of the drugs is in 0.1ng/mL between 0.5ng/mL.
The present invention is sample for other body fluid samples using saliva, and taking for saliva has acquisition convenient, not by
Time, place limitation；Easily received by subject, collection process does not invade personal privacy；Sampling process is easy to monitor, and can keep away
The advantages that exempting from the imitation behavior of sample.It is used as mixing drugs standard solution using containing 14 kinds of drugs standard items, it can be qualitative simultaneously
Or one of quantitative detection this 14 kinds of drugs or a variety of, sample pre-treatments are simple, detection time and workload are substantially reduced,
The technology of use have quickly, efficiently, the advantages such as sensitivity height, both can be qualitative or quantify.
Embodiment 1
A kind of detection method of human poisoning product, wherein drugs to be detected include 14 kinds, specially amphetamine, methylbenzene
Propylamine, 3,4- methylene benzylene chloride propylamine, ketamine, heroin, morphine, codeine, pethidine, methadone, sweet smell are too
Buddhist nun, 6- monoacetylmorphine, tetrahydrocannabinol, benzoyl ecgonine, cocaine, the detection method include:
The saliva 5mL that 5 normal adults flow out naturally is collected, is centrifuged 5 minutes after mixing, supernatant is taken, 10mL is added and goes
Ionized water, be vortexed concussion 15s, adds 30mL precipitating reagent, and be vortexed concussion 15s, and 3000rpm room temperature is centrifuged 1min, after taking supernatant
The mixed mark of drugs is added, makes the final concentration of 10ppb of every kind be added drugs, and using the mixing sample of acquisition as to test sample
This, simulates authentic sample, takes 100 μ L to mix sample and sample introduction bottle is added, spare.
Take 14 kinds of drugs standard items substances respectively, diluted step by step with deionized water, be configured to 0.1ng/mL, 0.5ng/mL,
The standard solution of 1.0ng/mL, 10ng/mL, 50ng/mL, 100ng/mL, then respectively by the mark of the respective concentration of 14 kinds of drugs
Quasi- solution mixing, it is spare so that the standard items mixed solution of 6 kinds of concentration is made.
It, will treated sample and the mixing drugs mark using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS)
Quasi- solution carries out Mass Spectrometer Method respectively, determines in the mass spectrogram of obtained sample and the mass spectrogram of the mixing drugs standard solution
There is following parent ion/daughter ion pair: the amphetamine: 136.1/91.1,136.1/119.1, the crystal methamphetamine:
150.2/91.1,150.2/119.1,3, the 4- methylene benzylene chloride propylamine: 194.1/163.1,194.1/
105.2, the ketamine: 238.1/125.2,238.1/220.1, the heroin: 370.2/328.2,370.2/268.2,
The morphine: 286.1/165.0,286.1/201.0, the codeine: 300.1/165.1,300.1/215.1, the piperazine replace
Pyridine: 248.1/174.1,248.1/220.1, the methadone: 310.2/265.2,310.2/265.2, the fentanyl:
337.2/188.1,337.2/105.1, the 6- monoacetylmorphine: 328.1/211.3,328.1/165.3, the tetrahydro are big
Numb phenol: 315.2/259.2,315.2/193.2, the benzoyl ecgonine: 290.1/168.1,290.1/105.2, it is described can
Cacaine: 304.1/182.1,304.1/150.2.Further, confirm the chromatographic peak of each pair of parent ion/daughter ion pair in the sample
Retention time with the corresponding chromatographic peak retention time relative error of the mixing drugs standard solution less than 2%, and the sample
Parent ion/the daughter ion of product to relative abundance than with mixing drugs standard solution relative abundance than consistent, as a result, really
There are aforementioned parent ion/daughter ions in the mixing drugs standard solution in the fixed sample to corresponding 14 kinds of drugs, from
And realize qualitative analysis；
Draw parent ion/daughter ion in standard curve, and the detection sample to peak area (select herein it is female from
Son/daughter ion pair are as follows: the amphetamine: 136.1/91.1, the crystal methamphetamine: 150.2/91.1,3, the 4- methylene
Benzylene chloride propylamine: 194.1/163.1, the ketamine: 238.1/125.2, the heroin: 370.2/328.2, institute
State morphine: 286.1/165.0, the codeine: 300.1/165.1, the pethidine: 248.1/174.1, the methadone:
310.2/265.2, the fentanyl: 337.2/188.1, the 6- monoacetylmorphine: 328.1/211.3, the tetrahydro hemp
Phenol: 315.2/259.2, the benzoyl ecgonine: 290.1/168.1, the cocaine: 304.1/182.1), and according to
The standard curve obtains the concentration of the sample, to carry out quantitative analysis.
Wherein, the testing conditions of the Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) are as follows:
Liquid phase column: ACE EXCEL2C18UPLC chromatographic column (2.1 × 50mm, 1.8 μm)；
Column temperature: 50 DEG C；
Mobile phase: A is the 5mmol/L ammonium formate solution of pH3.0, and B is 0.1% formic acid of volume fraction-acetonitrile solution；
Flow velocity: 500 μ L/min；
Sample volume: 10 μ L；
Ion source: it uses electrospray ionisation-positive ion mode (ESI+)；
Detection mode: multiple-reaction monitoring
Referring to Fig. 1~Figure 15, Fig. 1 is the mixing sample MRM map for being used to simulate authentic specimen that embodiment 1 obtains.Fig. 2
~Figure 15 is the standard curve of 14 kinds of drugs.
Further, according to standard curve and the parent ion/daughter ion measured to peak area, corresponding drugs in sample are calculated
Concentration.
Wherein, the detection limit of 14 kinds of drugs and quantitative limit are referring specifically to table 3.
The detection limit and quantitative limit of table 3:14 kind drugs
Quantitative detection result is as follows: amphetamine 6.46ppb, crystal methamphetamine 9.97ppb, 3,4-methylene dioxy methyl
Amphetamine 7.69ppb, ketamine 8.15ppb, heroin 6.28ppb, morphine 3.98ppb, codeine 6.72ppb, pethidine
10.16ppb, methadone 11.3ppb, fentanyl 9.47ppb, 6- monoacetylmorphine 4.85ppb, tetrahydrocannabinol 9.92ppb, benzene
Formyl ecgonine 9.58ppb, cocaine 10.26ppb.
Embodiment 2
A kind of detection method of human poisoning product, wherein the drugs are heroin, the detection method includes:
Sample treatment: at 5 points in afternoon collects the saliva 6mL that 6 normal adults flow out naturally, is centrifuged 5 minutes, takes after mixing
12mL deionized water is added in supernatant, and be vortexed concussion 15s, adds 18mL precipitating reagent, and be vortexed concussion 15s, 3000rpm room temperature from
Heart 5min takes the standard items of addition heroin after supernatant, makes the final concentration of 10ppb of theory of heroin be added, and to obtain
The mixing sample obtained simulates authentic sample, takes 150 μ L to mix sample and sample introduction bottle is added, spare.
Take 14 kinds of drugs standard items substances respectively, diluted step by step with deionized water, be configured to 0.1ng/mL, 0.5ng/mL,
The standard solution of 1.0ng/mL, 10ng/mL, 50ng/mL, 100ng/mL, then respectively by the mark of the respective concentration of 14 kinds of drugs
Quasi- solution mixing, it is spare so that the standard items mixed solution of 6 kinds of concentration is made.
It, will treated sample and the mixing drugs mark using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS)
Quasi- solution carries out Mass Spectrometer Method respectively, determines in the mass spectrogram of obtained sample and the mass spectrogram of the mixing drugs standard solution
There is following parent ion/daughter ion pair: the heroin: 370.2/328.2,370.2/268.2.Further, described in judgement
The corresponding chromatographic peak of the chromatographic peak retention time of each pair of parent ion/daughter ion pair and the mixing drugs standard solution in sample
Retention time relative error is less than 2%, and the parent ion/daughter ion of the sample is to relative abundance ratio and mixing drugs mark
There are the mothers in the mixing drugs standard solution in the sample than unanimously, determining as a result, for the relative abundance of quasi- solution
Ion/daughter ion is to corresponding drugs --- heroin, to realize qualitative analysis；
Draw parent ion/daughter ion in standard curve, and the detection sample to peak area (select herein it is female from
Son/daughter ion pair are as follows: 370.2/268.2), and the concentration of the sample is obtained according to the standard curve, to be quantified
Analysis.
Wherein, the testing conditions of the Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) are as follows:
Liquid phase column: ACE EXCEL2C18UPLC chromatographic column (2.1 × 50mm, 1.8 μm)；
Column temperature: 50 DEG C；
Mobile phase: A is the 5mmol/L ammonium formate solution of pH3.0, and B is 0.1% (volume fraction) formic acid-acetonitrile solution；
Flow velocity: 500 μ L/min；
Sample volume: 10 μ L；
Ion source: it uses electrospray ionisation-positive ion mode (ESI+)；
Detection mode: multiple-reaction monitoring
LC-MS/MS testing result see Figure 16~Figure 17, Figure 16 be embodiment 2 obtain be used to simulate the mixed of authentic specimen
The MRM map of sample is closed, Figure 17 is the standard curve of the heroin of production.According to standard curve and the parent ion/son measured from
For son to peak area, the concentration for calculating the heroin into sample is 8.553ppb.
It should be noted that being all the toxic sample of saliva of simulation, the saliva sample of 5 or 6 people in Examples 1 and 2
Mixing is to exclude individual difference.In addition, theoretically the concentration of every kind of drugs should in the testing result of Examples 1 and 2
For 10ppb, and saliva, referred to herein as matrix, the substance for detection are influential, thus the testing result of Examples 1 and 2
In error range.Wherein, influence of the matrix for detection target, referred to as matrix effect.For every kind of substance, matrix effect
It should be different.
Embodiment 3
A kind of detection method of human poisoning product, the detection method include:
Sample process: the saliva 2mL that a drug addict is flowed out naturally is collected when afternoon 6, is centrifuged 3 minutes, takes after mixing
4mL deionized water is added in supernatant, and be vortexed concussion 15s, adds 6mL precipitating reagent, and be vortexed concussion 15s, the centrifugation of 3000rpm room temperature
3min takes 1mL supernatant spare, takes 150 μ L samples that sample introduction bottle is added, to be checked；When acquiring saliva sample, while extracting vein
Blood 5mL, it is spare.
Take 14 kinds of drugs standard items substances respectively, diluted step by step with deionized water, be configured to 0.1ng/mL, 0.5ng/mL,
The standard solution of 1.0ng/mL, 10ng/mL, 50ng/mL, 100ng/mL, then respectively by the mark of the respective concentration of 14 kinds of drugs
Quasi- solution mixing, it is spare so that the standard items mixed solution of 6 kinds of concentration is made.
It, will treated sample and the mixing drugs mark using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS)
Quasi- solution carries out Mass Spectrometer Method respectively, determines in the mass spectrogram of obtained sample and the mass spectrogram of the mixing drugs standard solution
Whether following parent ion/daughter ion pair: the amphetamine: 136.1/91.1,136.1/119.1 is occurred, the crystal methamphetamine:
150.2/91.1,150.2/119.1,3, the 4- methylene benzylene chloride propylamine: 194.1/163.1,194.1/
105.2, the ketamine: 238.1/125.2,238.1/220.1, the heroin: 370.2/328.2,370.2/268.2,
The morphine: 286.1/165.0,286.1/201.0, the codeine: 300.1/165.1,300.1/215.1, the piperazine replace
Pyridine: 248.1/174.1,248.1/220.1, the methadone: 310.2/265.2,310.2/265.2, the fentanyl:
337.2/188.1,337.2/105.1, the 6- monoacetylmorphine: 328.1/211.3,328.1/165.3, the tetrahydro are big
Numb phenol: 315.2/259.2,315.2/193.2, the benzoyl ecgonine: 290.1/168.1,290.1/105.2, it is described can
Cacaine: 304.1/182.1,304.1/150.2.As a result, detecting parent ion/daughter ion pair of the ketamine: 238.1/
125.2,238.1/220.1.Further, judge in the sample chromatographic peak retention time of each pair of parent ion/daughter ion pair with
The corresponding chromatographic peak retention time relative error of the mixing drugs standard solution is less than 2%, and the mother of the sample
Ion/daughter ion is to relative abundance than, than consistent, being determined in the sample as a result, with the relative abundance of mixing drugs standard solution
There are the parent ion/daughter ions in the mixing drugs standard solution to corresponding drugs --- ketamine, to realize
Qualitative analysis；
Draw parent ion/daughter ion in standard curve, and the detection sample to peak area (select herein it is female from
Son/daughter ion obtains the concentration of the sample according to the standard curve to for 238.1/125.2), quantitatively to be divided
Analysis.
Wherein, the testing conditions of the Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) are as follows:
Liquid phase column: ACE EXCEL2C18UPLC chromatographic column (2.1 × 50mm, 1.8 μm)；
Column temperature: 50 DEG C；
Mobile phase: A is the 5mmol/L ammonium formate solution of pH3.0, and B is 0.1% (volume fraction) formic acid-acetonitrile solution；
Flow velocity: 500 μ L/min；
Sample volume: 10 μ L；
Ion source: it uses electrospray ionisation-positive ion mode (ESI+)；
Detection mode: multiple-reaction monitoring
Blood sample detection uses gas chromatography-mass spectrometry, with reference to 2016 judicial expertise technical specification (SF/Z
JD0107004-2016), specifically: it takes blood sample 2mL to be placed in 10mL tool plug centrifuge tube, it is molten that 10% sodium hydroxide is added
Liquid 0.2mL is extracted, vortex mixed, centrifugation with ether 3mL, organic layer is shifted into another centrifuge tube, in about 60 DEG C of water-baths
It volatilizes, residue is dissolved with 50 μ L methanol, and 1 μ L is taken to analyze into Gc/ms Analyser.
LC-MS/MS testing result is shown in that attached drawing, Figure 18 are the MRM maps of the sample of embodiment 3, and Figure 19 is prepared
The standard curve of ketamine.As a result, LC-MS/MS detects the concentration 4.68ppb of ketamine in sample, prior art GC-MS
Detect the concentration 4.8ppb of ketamine in blood sample, two kinds of detection technique relative errors are no more than 20%, coincidence statistics
It is required that.
Above-described embodiment is preferred embodiments of the present invention, but the embodiment of the present invention is not by the limit of above-described embodiment
System, above embodiments are only for interpreting the claims.Right protection scope of the present invention is not limited to specification.It is any ripe
Know those skilled in the art within the technical scope of the present disclosure, the variation or replacement that can be readily occurred in all are wrapped
Containing within protection scope of the present invention.
Claims (10)
1. a kind of detection method of human poisoning product, which comprises the following steps:
A series of mixing drugs standard solution of gradient concentrations is prepared using 14 kinds of drugs standard items；
Using Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS), sample and the mixing drugs standard solution are subjected to matter respectively
Spectrum detection, based on Mass Spectrometer Method as a result, when having the following conditions at the same time, determines that there are the mixing drugs marks in the sample
One of quasi- solution or a variety of drugs, to realize qualitative analysis: (1) in the mass spectrogram of the sample and the mixing drugs
There is the corresponding parent ion/daughter ion pair of at least one of identical 14 kinds of drugs in the mass spectrogram of standard solution；(2)
The chromatographic peak retention time of each pair of parent ion/daughter ion pair present in the sample and pair for mixing drugs standard solution
The chromatographic peak retention time relative error answered is less than 2%；(3) each pair of parent ion/daughter ion pair existing for the sample is opposite
Abundance than with the relative abundance of the corresponding parent ion/daughter ion pair of the mixing drugs standard solution than consistent；
Standard curve, and parent ion/daughter ion pair peak area of the drugs present in the detection sample are drawn, and
And the concentration of the sample is obtained according to the standard curve, with quantitative analysis,
Optionally, the sample source is in people's saliva,
Optionally, the sample is by pretreatment.
2. the detection method of human poisoning product as described in claim 1, which is characterized in that the liquid chromatography-tandem mass spectrometry
The determination condition of method (LC-MS/MS) includes: that liquid phase column is reverse chromatograms column；Column temperature is 40 DEG C~55 DEG C；Mobile phase includes flowing
Phase A and Mobile phase B, the mobile phase A are the ammonium formate solution of 2~10mmol/L, and the Mobile phase B is formic acid-acetonitrile solution,
The ammonium formate solution and the volume ratio of the formic acid-acetonitrile solution are 1:15~15:1；Flow velocity is 400~600 μ L/min.
3. the detection method of human poisoning product as described in claim 1, which is characterized in that the pretreatment includes: will be described
Saliva is centrifuged after mixing, and takes supernatant, and deionized water is added, and be vortexed concussion, and precipitating reagent is added, be vortexed again for concussion, be centrifuged with
And take supernatant.
4. the detection method of human poisoning product as claimed in claim 3, which is characterized in that the precipitating reagent is selected from sulfosalisylic
Acid solution, urea or guanidine hydrochloride.
5. the detection method of human poisoning product as claimed in claim 3, which is characterized in that the saliva, the deionized water
Volume ratio with the precipitating reagent is 1:1:1-1:2:3.
6. the detection method of human poisoning product as described in claim 1, which is characterized in that with the detection of the human poisoning product
The drugs of method detection include amphetamine, crystal methamphetamine, 3,4- methylene benzylene chloride propylamine, ketamine, Hai Luo
Cause, codeine, pethidine, methadone, fentanyl, 6- monoacetylmorphine, tetrahydrocannabinol, benzoyl ecgonine, can block morphine
One of cause is a variety of.
7. the detection method of human poisoning product as described in claim 1, which is characterized in that the liquid chromatography-tandem mass spectrometry
The determination condition of method (LC-MS/MS) further includes that ion source is electrospray ionisation-positive ion mode (ESI+)；Detection mode is more
Reaction monitoring (MRM)；The pressure of gas curtain gas is 10-55Psi；Collision atmospheric pressure is 0-12Psi；Atomization temperature is 0-550 DEG C；Mist
Change atmospheric pressure is 0-90Psi.
8. the detection method of human poisoning product as claimed in claim 6, which is characterized in that in carrying out the qualitative analysis,
Corresponding parent ion/the daughter ion of each drugs is to being all made of two pairs in 14 kinds of drugs, wherein two couples of mothers of every kind of drugs
Ion/daughter ion is to being respectively as follows: the amphetamine: 136.1/91.1,136.1/119.1, the crystal methamphetamine: 150.2/
91.1,150.2/119.1,3, the 4- methylene benzylene chloride propylamine: 194.1/163.1,194.1/105.2, the chlorine
Amine ketone: 238.1/125.2,238.1/220.1, the heroin: 370.2/328.2,370.2/268.2, the morphine:
286.1/165.0,286.1/201.0, the codeine: 300.1/165.1,300.1/215.1, the pethidine: 248.1/
174.1,248.1/220.1, the methadone: 310.2/265.2,310.2/265.2, the fentanyl: 337.2/188.1,
337.2/105.1, the 6- monoacetylmorphine: 328.1/211.3,328.1/165.3, the tetrahydrocannabinol: 315.2/
259.2,315.2/193.2, the benzoyl ecgonine: 290.1/168.1,290.1/105.2, the cocaine: 304.1/
182.1、304.1/150.2。
9. the detection method of human poisoning product as described in claim 1, which is characterized in that in carrying out the quantitative analysis,
For the drugs present in the sample, select two pairs of parent ion/daughter ions at least one of detection peak area,
In, two pairs of parent ion/daughter ions of every kind of drugs are described to being respectively as follows: the amphetamine: 136.1/91.1,136.1/119.1
Crystal methamphetamine: 150.2/91.1,150.2/119.1,3, the 4- methylene benzylene chloride propylamine: 194.1/163.1,
194.1/105.2, the ketamine: 238.1/125.2,238.1/220.1, the heroin: 370.2/328.2,370.2/
268.2, the morphine: 286.1/165.0,286.1/201.0, the codeine: 300.1/165.1,300.1/215.1, institute
State pethidine: 248.1/174.1,248.1/220.1, the methadone: 310.2/265.2,310.2/265.2, the sweet smell is too
Buddhist nun: 337.2/188.1,337.2/105.1, the 6- monoacetylmorphine: 328.1/211.3,328.1/165.3, the tetrahydro
Cannabinol: 315.2/259.2,315.2/193.2, the benzoyl ecgonine: 290.1/168.1,290.1/105.2, it is described
Cocaine: 304.1/182.1,304.1/150.2.
10. the detection method of human poisoning product as described in claim 1, which is characterized in that it is described fixed to carry out in the drugs
Measure in fixed, the range of detection limit in 0.02ng/mL between 0.14ng/mL, the range of quantitative limit 0.1ng/mL extremely
Between 0.5ng/mL.
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