CN1916602A - Capillary electrophoresis method for detecting medications and poisons in blood and urine at the same time - Google Patents
Capillary electrophoresis method for detecting medications and poisons in blood and urine at the same time Download PDFInfo
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- CN1916602A CN1916602A CN 200510028952 CN200510028952A CN1916602A CN 1916602 A CN1916602 A CN 1916602A CN 200510028952 CN200510028952 CN 200510028952 CN 200510028952 A CN200510028952 A CN 200510028952A CN 1916602 A CN1916602 A CN 1916602A
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Abstract
A capillary cataphoresis method for detecting multiple medicinal toxic in blood and in urine simultaneously includes carrying out pretreatment by using similar solid phase to extract basic and acidic medicinal toxic, applying high efficiency of capillary cataphoresis detection and internal standard means of quantitative for enabling to analyze out 55 types of medicinal toxics contained possibly in one blood sample or in one urine sample within dozens of ten minutes.
Description
Technical field
The present invention relates to a kind of method that detects multiple medicine and poisonous substance in blood or the urine simultaneously, more specifically relate to a kind of high performance capillary electrophoresis (HPCE) method of can be simultaneously 55 kinds of medicines in blood or the urine and poisonous substance being carried out quantitative measurement.
Background technology
The main method that medicine and toxicological analysis adopt at present has: vapor-phase chromatography (GC), gas chromatography mass spectrometry method (GC-MS), high performance liquid chromatography (HPLC), thin-layered chromatography (TLC) and Enzyme-multiplied immune technique analysis (EMIT) etc.HPCE is used for the analysis of medicine and poisonous substance, had obtained development faster in recent years.Domestic and foreign literature has been reported the application of HPCE in toxicological analysis in succession, but mainly concentrates in the research of same class medicine poisonous substance or a few kind potpourri.Zhang Yahai etc. use HPCE to detect the content [Zhang Yahai etc., contemporary Chinese is used pharmaceutical journal, 2000,17 (1)] of morphine in the heroin addict urine; Wang Bo etc. are to studying with capillary zone electrophoresis separation determination amphetamine and meth; Use HPCE such as Gianpiero are equipped with diode array detector amphetamine-type in the whole blood are detected [Gianpiero Boatto, MariaVirginia Faedda, Amedeo Pau, Journal of Pharmaceutical and Biomedical Analysis, 2002; 29:1073-1080]; Carolien etc. have studied and have used different CE patterns that [Carolien M.Boone, Jan Willem Souma, Jan Piet Franke, Forensic Science International, 2001 are analyzed in human blood, the screening of urine Chinese medicine poisonous substance; 121:89-96]; Walker etc. utilize capillary zone electrophoresis that forbidden drug has been carried out screening and quantitative examination [J.A.Walker, et al.J.Forensic.Sci., 1996,41 (5): 824-829].
These bibliographical informations use different analytical approachs to all kinds of medicine poisonous substances, have very strong specific aim, more are applicable to the analysis of known class medicine poisonous substance.But it is, relatively poor to the practicality and the comparability of unknown medicine toxicological analysis because of it lacks versatility.In the work for inspection of reality, because what relate in a large number is unknown case, its target analytes usually can not be clearly sure in advance, so, be badly in need of wanting a kind of HPCE analytical approach that can fast, effectively distinguish variety classes medicine poisonous substance, with existing HPLC, analysis technology such as GC are replenished mutually, increase detects probability, reduces the generation of omission situation, better more effectively unknown medicine poisonous substance is carried out Analysis and Identification.
Summary of the invention
The object of the present invention is to provide a kind of high performance capillary electrophoresis analysis method that can detect multiple medicine toxic content in blood or the urine effectively.
The present invention adopts capillary zone electrophoresis, and (capillary zone electrophoresis CZE) analyzes different types of 55 kinds of medicine poisonous substances in human whole blood and the urine.For acid, alkaline medicine poisonous substance, use same pre-service and deposition condition separately, adopt inner mark method ration, with butalbital (Butalbital) or doxapram (Doxapram) as interior mark.
Different types of 55 kinds of medicine poisonous substances comprise:
1, opium and synthetic material thereof: pholcodine (Pholcodine), thebaine (Thebaine), codeine phosphate (CodeinePhosphate), morphine sulfate (Morphine Sulfate), O
6-monoacetylmorphine (O
6-monoacetylmorphine), Heroinhydrochloride (Heroin Hydrochloride), coscopin (Noscapine), pethidine hydrochloride (Pethidine Hydrochloride), methadone hydrochloride (Methadone Hydrochloride), acetyl codeine (Acetylcodeine), O
3-monoacetylmorphine (O
3-monoacetylmorphine), fentanyl citrate (Fentanyl Citrate), papaverine hydrochloride (PapaverineHydrochloride), diphenoxylate hydrochloride (Diphenoxylate Hydrochloride), hydrochloric acid Lepetan (BuprenorphineHydrochloride), naloxone hydrochloride (Naloxone Hydrochloride).
2, cocaines and synthetic substitute: cocainehydrochloride (Cocaine Hydrochloride), totokaine (Tetracaine), procaine hydrochloride (Procaine Hydrochloride), lidocaine (Lidocaine), Bupivacaine (Bupivacaine).
3, amphetamine and admixture: amphetamine sulfate (Amphetamine Sulfate), hydrochloride methyl amphetamine (Methamphetamine Hydrochloride), 3.4-methylene dioxy base amphetamine (MDA), 3,4-methylene dioxy ylmethyl amphetamine hydrochloride (MDMA Hydrochloride), ketamine (Ketamine).
4, tricyclic antidepressant and phenothiazines antipsychotic drug: fenazil (Promethazine), Clozapine (Clozapine), perphenazine (Perphenazine), triperazine (Trifluoperazine), fluphenazine hydrochloride (Fluphenazine Hydrochloride), chlorpromazine (Chlorpromazine), Chlorprothixene (Chlorprothixene), haloperole (Haloperidol), Impamin (Imipramine Hydrochloride), doxepin hydrochloride (Doxepin Hydrochloride).
5, benzene a pair of horses going side by side diazepine class: diazepam (Diazepam), midazolam (Midazolam), Flurazepam (Flurazepam), remove first diazepam (Nordiazepam).
6, alkaloids and composite: pseudoephedrine hydrochloride (Pseudoephedrine Hydrochloride), ephedrine hydrochloride (Ephedrine Hydrochloride), phenylpropanolamine HC1 (Phenylpropanolamine Hydrochloride), strychnia (Brucine), strychnine (Strychnine), atropine sulfate (Atropine Sulfate), Anisodamine (AnisodamineHydrobromide), scopolamine hydrobromide (Scopolamine Hydrobromide), chloroquine (Chloroquine), quinine sulfate (Quinine Sulfate).
7, barbiturates: yellow Jackets (Pentobarbital Sodium), barbose (Secobarbital Sodium), amytal (Amobarbital), barbital (Barbital), phenobarbital (Phenobarbital).
The inventive method may further comprise the steps:
One, sample preparation:
By solid-phase extraction column operation instruction method pillar is activated and (to use methyl alcohol usually, each 1mL of water crosses post) after get urine sample 1mL or diluting blood sample liquid 1mL upper prop, again with the aqueous solution 1mL drip washing pillar that contains small amount of acid (as acetate) or small amount of alkali (as ammoniacal liquor) and a small amount of organic solvent (as methyl alcohol), pillar is drained back appropriate amount of organic wash-out (available ethyl acetate or methylene chloride 1mL), to add 20 μ L 1%HCL methanol solutions in the alkalescence medicine poisonous substance eluent, the organic solvent eluent be volatilized the back dissolve the back sample introduction with 0.02-0.1mL water-methanol (4: 1).
Inner mark solution can adopt and contain butalbital 0.01-0.1mgmL in the above-mentioned preprocess method
-1Or doxapram 0.01-0.1mgmL
-1Methanol solution, consumption is generally at 5-50ul, in urine sample and the blood sample in target sample introduction concentration can be controlled in 0.05mgmL
-1Or 0.025mgmL
-1About.
Containing sour leacheate is acetate, hydrochloric acid or phosphoric acid, and containing the alkali leacheate is ammoniacal liquor, NaOH or sodium carbonate, the organic solvent leacheate is methyl alcohol, ethanol or acetonitrile.
The sample of selecting for use is a whole blood, adds acid when handling whole blood, as phosphoric acid, sulfuric acid or oxalic acid.
Two, Capillary Electrophoresis parameter:
1, damping fluid: 150mmolL
-1Phosphate+20% methyl alcohol (pH 2.38) is analyzed alkaline medicine poisonous substance; 100mmolL
-1Borate+15% methyl alcohol (pH 8.5) is analyzed acid medicine poisonous substance.
2, sampling condition: coating quartz capillary column (75 μ m * 50.2cm, effectively separation length be 40cm) not, pressure sample introduction 0.5psi * 10s; Separation voltage is 16kv; 25 ℃ of column temperatures; Detect that wavelength is respectively 200,210,238nm.Each start back is washed 10min respectively with 1molL-1 sodium hydroxide solution, water and running buffer, washes 3min with running buffer between 2 analyses.
Three, density calculating method
Calculate the concentration of these 55 kinds of medicine poisonous substances in urine or the blood with peak area or peak height method by internal standard method.
Beneficial effect
1, the inventive method sample treatment is easy and simple to handle, and urine sample and blood sample impurity are noiseless to the detection by quantitative of medicine poisonous substance.
2, the inventive method is strong, highly sensitive to the detection selectivity of sample, and every methodology index all can satisfy the needs of actual inspection case easy, reliably.
Description of drawings
Fig. 1 is the separate colors spectrogram of 21 kinds of alkaline medicine poisonous substances
1. chloroquine 2. pholcodines 3. amphetamines 4. meth 5.MDA 6.MDMA 7. pseudoephedrines 8. ephedrines 9. ketamines 10. pethidines 11. fenazils 12. imipramines 13. Chlorprothixenes 14. thebaine 15. codeines 16. morphine 17.O
6-monoacetylmorphine 18. heroin 19. coscopins 20. haloperole 21. diphenoxylates
Fig. 2 is the separate colors spectrogram of 20 kinds of alkaline medicine poisonous substances
1. chloroquine 2. pholcodines 3. quinines 4. Clozapines 5. procaines 6. ketamines 7. totokaine 8. cocaines 9. lidocaines 10. doxepins 11. methadones 12. codeines 13. Bupivacaines 14. acetyl codeine 15.O
3-monoacetylmorphine 16. fentanyls 17. coscopins 18. haloperole 19. strychnias 20. Lepetans
Fig. 3 is the separate colors spectrogram of 18 kinds of alkaline medicine poisonous substances
1. chloroquine 2. pholcodines 3. amphetamines 4. meth 5.MDMA 6. phenylpropanolamines 7. ephedrines 8. ketamines 9. triperazines 10. hyoscines 11. atropines 12. codeines 13. anisodamines 14. Allylnoroxymorphones 15. papaverines 16. coscopins 17. haloperole 18. diazepams
Fig. 4 is the separate colors spectrogram of 16 kinds of alkaline medicine poisonous substances
1. chloroquine 2. pholcodines 3. quinines 4. Clozapines 5. procaines 6. ketamines 7. perphenazine 8. fluphenazinum 9. chlorpromazines 10. strychnines 11. remove first diazepam 12. Flurazepams 13. midazolams 14. Allylnoroxymorphones 15. strychnias 16. diazepams
Fig. 5 is the separate colors spectrogram of 5 kinds of acid medicine poisonous substances
1. amobarbital 2. quinalbarbitones 3. amytal 4. barbitals 5. phenobarbitals
Fig. 6 is the chromatogram of embodiment 2.
1：MDA
Fig. 7 embodiment 3 chromatograms
1: meth, 2:MDMA, 3: ketamine
Fig. 8 is the chromatogram of embodiment 4
1: morphine
1: lidocaine
Figure 10 is the chromatogram of embodiment 6
1: doxepin
Figure 11 embodiment 7 chromatograms
1: phenobarbital
Embodiment
The present invention is further elaborated below in conjunction with specific embodiment, but do not limit the present invention.
1 material
1.1 instrument Beckman P/ACE MDQ capillary electrophoresis apparatus (U.S. Beckman company); Coating quartz capillary column (75 μ m * 50.2cm, effectively separation length is 40cm, Beckman company) not; Oasis HLB post (1mL/30mg, waters company); Vortex mixer XW-80A; Electric-heated thermostatic water bath.
1.2 reagent and medicine
Opium and synthetic material thereof: pholcodine (Pholcodine), thebaine (Thebaine), codeine phosphate (CodeinePhosphate), morphine sulfate (Morphine Sulfate), O
6-monoacetylmorphine (O
6-monoacetylmorphine), Heroinhydrochloride (Heroin Hydrochloride), coscopin (Noscapine), pethidine hydrochloride (Pethidine Hydrochloride), methadone hydrochloride (Methadone Hydrochloride), acetyl codeine (Acetylcodeine), O
3-monoacetylmorphine (O
3-monoacetylmorphine), fentanyl citrate (Fentanyl Citrate), papaverine hydrochloride (PapaverineHydrochloride), diphenoxylate hydrochloride (Diphenoxylate Hydrochloride), hydrochloric acid Lepetan (BuprenorphineHydrochloride), naloxone hydrochloride (Naloxone Hydrochloride).
Cocaines and synthetic substitute: cocainehydrochloride (Cocaine Hydrochloride), totokaine (Tetracaine), procaine hydrochloride (Procaine Hydrochloride), lidocaine (Lidocaine), Bupivacaine (Bupivacaine).
Amphetamine and admixture: amphetamine sulfate (Amphetamine Sulfate), hydrochloride methyl amphetamine (Methamphetamine Hydrochloride), 3.4-methylene dioxy base amphetamine (MDA), 3.4-methylene dioxy ylmethyl amphetamine hydrochloride (MDMAHydrochloride), ketamine (Ketamine).
Phenothiazines and tricyclic antidepressant: fenazil (Promethazine), Clozapine (Clozapine), perphenazine (Perphenazine), triperazine (Trifluoperazine), fluphenazine hydrochloride (Fluphenazine Hydrochloride), chlorpromazine (Chlorpromazine), Chlorprothixene (Chlorprothixene), haloperole (Haloperidol), Impamin (Imipramine Hydrochloride), doxepin hydrochloride (Doxepin Hydrochloride).
Benzene a pair of horses going side by side diazepine class: diazepam (Diazepam), midazolam (Midazolam), Flurazepam (Flurazepam), remove first diazepam (Nordiazepam).
Alkaloids and composite: pseudoephedrine hydrochloride (Pseudoephedrine Hydrochloride), ephedrine hydrochloride (Ephedrine Hydrochloride), phenylpropanolamine HC1 (Phenylpropanolamine Hydrochloride), strychnia (Brucine), strychnine (Strychnine), atropine sulfate (Atropine Sulfate), Anisodamine (AnisodamineHydrobromide), scopolamine hydrobromide (Scopolamine Hydrobromide), chloroquine (Chloroquine), quinine sulfate (Quinine Sulfate).
Barbiturates: yellow Jackets (Pentobarbital Sodium), barbose (Secobarbital Sodium), amytal (Amobarbital), barbital (Barbital), phenobarbital (Phenobarbital).
55 kinds of reference substances and interior mark doxapram (Doxapram), butalbital (Butalbital) are provided by Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
Ethyl acetate (chemical reagent company limited in Shanghai analyzes pure); Methyl alcohol (magnificent forever reagent subsidiary factory of chemicals factory of Shanghai City Fudan University, chromatographically pure); Ammoniacal liquor (Taicang is Ward kind chemical reagent work forever, analyzes pure); Hydrochloric acid (chemical plant, Kingsoft is analyzed pure); Phosphoric acid (the inferior chemical plant that shakes is analyzed pure); Sodium dihydrogen phosphate (chemical plant, Kingsoft, Shantou is analyzed pure); Borax (Shanghai Ling Feng chemical reagent company limited analyzes pure); Boric acid (the virtuous chemical reagents corporation in east, Shanghai); The Millipore ultrapure water.
1.3 storing solution
1.3.1 reference substance storing solution alkalescence medicine poisonous substance is made into 1.0mgmL with methyl alcohol
-1Reference substance solution, be divided into four groups by Fig. 1～Fig. 4, equal-volume mixes in the time of quantitatively, being diluted to the concentration of mixing reference substance solution with methyl alcohol is 0.05mgmL
-1(first group does not comprise haloperole).
Acid medicine poisonous substance is made into 1.0mgmL with methyl alcohol
-1Reference substance solution, equal-volume mixes, being diluted to the concentration of mixing reference substance solution with methyl alcohol is 0.10mgmL
-1
1.3.2 interior mark storing solution
Storing solution A: doxapram is made into 1.0mgmL with methyl alcohol
-1Solution is diluted to 0.05mgmL with methyl alcohol
-1
Storing solution B: doxapram is made into 1.0mgmL with methyl alcohol
-1Solution, use methyl alcohol: water (1: 4) is diluted to 0.025mgmL
-1
Storing solution C: butalbital is made into 1.0mgmL with methyl alcohol
-1Solution is diluted to 0.1mgmL with methyl alcohol
-1
Storing solution D: butalbital is made into 1.0mgmL with methyl alcohol
-1Solution, use methyl alcohol: water (1: 4) is diluted to 0.05mgmL
-1
2 methods
2.1 deposition condition
Use CZE1:150mmolL
-1Phosphate+20% methyl alcohol (pH 2.38) is analyzed alkaline medicine poisonous substance; CZE2:100mmolL
-1Borate+15% methyl alcohol (pH 8.5) is analyzed acid medicine poisonous substance.Sampling condition: pressure sample introduction 0.5psi * 10s; Separation voltage is 16kv; 25 ℃ of column temperatures; Detect that wavelength is respectively 210,238nm.Use 1molL after each start
-1Sodium hydroxide solution, water and running buffer wash 10min respectively, wash 3min with running buffer between 2 analyses.Use 1molL before the shutdown
-1Sodium hydroxide solution, water wash 10min respectively.
2.2 sample preparation
1, activation extraction column
Use methyl alcohol, each 1mL of water crosses post
2, add interior mark
The a urine sample:
For acid medicine poisonous substance: add 0.1mgmL
-1 Butalbital methanol solution 10 μ L;
For alkaline medicine poisonous substance: add 0.05mgmL
-1Doxapram methanol solution 25 μ L.
The b whole blood:
Get the 0.5mL whole blood, water 1.5mL dilution adds 20 μ L phosphoric acid again.
For acid medicine poisonous substance: add 0.1mgmL
-1 Butalbital methanol solution 20 μ L;
For alkaline medicine poisonous substance: add 0.05mgmL
-1 Doxapram methanol solution 10 μ L.
3, go up sample
The a urine sample:
Get 1mL and go up sample.
The b whole blood:
Get sample on the 2mL whole blood dilution.
4, clean
The a urine sample:
For acid medicine poisonous substance: the first step: 1mL contains 2% acetic acid and 5% methanol in water; Second step: 1mL contains 5% methanol in water.
For alkaline medicine poisonous substance: the first step: 1mL contains 2% ammoniacal liquor and 5% methanol in water; Second step: 1mL contains 5% methanol in water.
The b whole blood:
For acid medicine poisonous substance: the first step: 1mL contains 2% acetic acid and 5% methanol in water; Second step: 1mL normal hexane; The 3rd step: 1mL contains 5% methanol in water.
For alkaline medicine poisonous substance: the first step: 1mL contains 2% ammoniacal liquor and 5% methanol in water; Second step: 1mL normal hexane; The 3rd step: 1mL contains 5% methanol in water.
5, centrifugal
With the centrifugal 3000rpm of extraction column, 5min.
6, wash-out
The a urine sample:
For acid medicine poisonous substance: select for use the 1mL methylene chloride as eluting solvent;
For alkaline medicine poisonous substance: select for use 1mL ethyl acetate as eluting solvent.
The b blood sample:
All medicine poisonous substances all select for use 1mL ethyl acetate-methyl alcohol (12: 1) as eluting solvent.
7, the adding of hydrochloric acid
Wash-out finishes alkaline medicine poisonous substance, adds 20 μ L 1%HCL methanol solutions in eluent.
8, dry up and constant volume
Eluent dries up under 55 ℃ of airflows, and with methanol-water (1: 4) constant volume, volume is: urine sample 50 μ L, blood neutral and alkali medicine 20 μ L, acidic drug 100 μ L.Sample introduction.
2.3 working curve
For alkaline medicine poisonous substance, prepare variable concentrations urine medicine and blood drug solns respectively, by the operation of 2.2 sample preparation methods.
For acid medicine poisonous substance, prepare variable concentrations urine medicine, blood drug solns respectively, by the operation of 2.2 sample preparation methods.
Ratio (Y) with medicine poisonous substance peak area and interior mark peak area is mapped to blood, urine Chinese medicine toxic concentration (X), gets the regression equation and the related coefficient of medicine poisonous substance.
2.4 absolute recovery
For alkaline medicine poisonous substance, get and mix stock solution in right amount in test tube at the bottom of the tool plug tip, dry up the back and respectively add blank urine 1.0mL or whole blood dilution 2mL (the 0.5mL whole blood dilutes with 1.5mL water), whole blood adds 20 μ L phosphoric acid again, be made into urine, the blood drug solns of high, medium and low three concentration, by 2.2 sample preparation methods (not adding interior mark) operation, add mark storing solution B in 50 μ L and the 20 μ L after drying up respectively, be transferred to micro-sampling pipe sample introduction.
For acid medicine poisonous substance, get and mix stock solution in right amount in test tube at the bottom of the tool plug tip, dry up the back and respectively add blank urine 1.0mL or whole blood dilution 2mL (the 0.5mL whole blood dilutes with 1.5mL water), whole blood adds 20 μ L phosphoric acid again, be made into urine, the blood drug solns of high, medium and low three concentration, by 2.2 sample preparation methods (not adding interior mark) operation, add mark storing solution D in 50 μ L and the 100 μ L after drying up respectively, be transferred to micro-sampling pipe sample introduction.
Other gets and mixes the solution that reference substance is made into respective concentration, and direct injected as standard, compares the calculating absolute recovery with the ratio of 2 groups of medicine poisonous substance peak areas and interior mark peak area.
2.5 relative recovery and precision
For alkaline medicine poisonous substance, it is an amount of to get the mixing stock solution, mark storing solution A:25 μ L and 10 μ L are in test tube at the bottom of the tool plug tip in adding respectively, add blank urine 1.0mL and whole blood dilution 2mL (the 0.5mL whole blood dilutes with 1.5mL water) after drying up respectively, the whole blood dilution adds 20 μ L phosphoric acid again, is made into urine, the blood drug solns of high, medium and low three concentration; By the operation of 2.2 sample preparation methods.
For acid medicine poisonous substance, it is an amount of to get the mixing stock solution, mark storing solution C:10 μ L and 20 μ L are in test tube at the bottom of the tool plug tip in adding respectively, add blank urine 1.0mL and whole blood dilution 2mL (the 0.5mL whole blood dilutes with 1.5mL water) after drying up respectively, whole blood adds 20 μ L phosphoric acid again, is made into urine, the blood drug solns of high, medium and low three concentration; By the operation of 2.2 sample preparation methods.
At last with the ratio substitution working curve equation of sample with interior target peak area, calculate recovery rate.Each concentration in a few days replication gets withinday precision 3 times, and METHOD FOR CONTINUOUS DETERMINATION 3d gets day to day precision.
2.6 detectability
Get the medicine poisonous substance of different amounts, volatilize solvent methanol, add urine 1mL or whole blood dilution 2mL (the 0.5mL whole blood dilutes with 1.5mL water), whole blood adds 20 μ L phosphoric acid again, by the operation of 2.2 sample treatments, sample introduction.
3 results
3.1 separating resulting
Because alkaline medicine poisonous substance involves a wide range of knowledge, kind is many, and quantity is big, and desire is separated relatively difficulty with all medicine poisonous substances in once analyzing, and alkaline medicine poisonous substance is divided into four groups, and under selected deposition condition, each component reaches baseline separation.And analysis speed is fast, can finish analysis in 18.5min.Acid medicine poisonous substance is less, is mainly barbiturates, can finish analysis in the 8.0min clock.
Under two deposition conditions, the impurity in blank urine, the blood sample is noiseless substantially, and each is organized medicine poisonous substance separate colors spectrogram and sees Fig. 1,2,3,4,5.
3.2 qualitative index
Mainly adopt relative migration time (rt according to the capillary electrophoresis separation characteristics
m), different ratio of peak (rh) under the wavelength and the ultraviolet spectrogram of detecting be as the component qualitative index.Each medicine poisonous substance rt under respective conditions
mSee Table 1 with the rh value.
Table 1-1 alkalescence medicine poisonous substance is with respect to interior target transit time and ratio of peak separately
| Medicine name | rt m(X±SD，min) | rh H 200/H 210 |
| Chloroquine pholcodine amphetamine meth quinine MDA MDMA Clozapine pseudoephedrine | 0.546±0.0009 0.561±0.0006 0.571±0.0028 0.584±0.0027 0.589±0.0009 0.618±0.0014 0.625±0.0024 0.630±0.0011 0.635±0.0024 | 0.700±0.0021 0.954±0.0089 1.413±0.0030 1.422±0.0079 0.878±0.0052 4.170±0.0033 4.033±0.0038 1.032±0.0030 1.309±0.0160 |
| Phenylpropanolamine ephedrine procaine ketamine totokaine pethidine cocaine fenazil perphenazine triperazine imipramine lidocaine doxepin hyoscine fluphenazinum Chlorprothixene chlorpromazine methadone thebaine atropine codeine morphine Bupivacaine strychnine anisodamine midazolam codeine O3-monoacetylmorphine O 6-monoacetylmorphine Allylnoroxymorphone papaverine fentanyl heroin nordiazepam coscopin | 0.638±0.0012 0.649±0.0023 0.663±0.0012 0.690±0.0020 0.722±0.0032 0.745±0.0015 0.747±0.0020 0.751±0.0019 0.755±0.0015 0.756±0.0012 0.765±0.0018 0.766±0.0004 0.776±0.0006 0.776±0.0003 0.778±0.0014 0.778±0.0028 0.794±0.0022 0.803±0.0005 0.804±0.0017 0.805±0.0006 0.827±0.0016 0.848±0.0015 0.850±0.0043 0.851±0.0006 0.853±0.0007 0.856±0.0008 0.866±0.0001 0.884±0.0002 0.886±0.0012 0.889±0.0014 0.897±0.0023 0.898±0.0004 0.908±0.0010 0.913±0.0019 0.928±0.0007 | 1.365±0.0130 1.376±0.0040 2.427±0.0067 2.270±0.0057 2.892±0.0140 1.843±0.0041 4.921±0.0284 1.394±0.0015 1.223±0.0086 1.297±0.0047 1.316±0.0043 1.809±0.0095 1.125±0.0009 1.797±0.0020 1.340±0.0106 1.156±0.0024 1.213±0.0131 1.771±0.0051 1.338±0.0017 1.793±0.0200 0.964±0.0008 1.009±0.0007 1.778±0.0012 1.153±0.0037 1.914±0.0105 1.149±0.0053 0.970±0.0026 1.173±0.0075 1.038±0.0012 1.418±0.0028 1.929±0.0095 1.591±0.0026 1.257±0.0043 1.326±0.0048 0.700±0.0032 |
| Mark strychnia Lepetan diazepam diphenoxylate in the Flurazepam haloperole | 0.955±0.0054 0.963±0.0004 1.000±0.0000 1.024±0.0008 1.042±0.0004 1.074±0.0079 1.076±0.0004 | 1.386±0.0053 1.873±0.0044 1.903±0.0085 1.088±0.0110 0.674±0.0052 1.367±0.0040 1.928±0.0200 |
The acid medicine poisonous substance of table 1-2 is with respect to interior target transit time and ratio of peak separately
| Medicine name | rt m(X±SD，min) | rh H 200/H 238 |
| Mark barbital phenobarbital in the amobarbital quinalbarbitone amytal | 0.971±0.0015 0.933±0.0013 0.955±0.0013 1.000±0.0000 1.030±0.0012 1.086±0.0008 | 3.038±0.0024 3.021±0.0091 2.749±0.0037 2.500±0.0046 2.711±0.0200 3.606±0.0230 |
3.3 working curve and detectability
The working curve and the detectability of each medicine poisonous substance see Table 2.
The working curve and the detectability of table 2 blood, urine Chinese medicine poisonous substance
| Medicine name | The range of linearity (urine)/ngmL -1 | Linear equation (urine) | Related coefficient (urine) | Detectability (urine) ngmL -1 | The range of linearity (blood)/ngmL -1 | Linear equation (blood) | Related coefficient (blood) | Detectability (blood) ngmL -1 |
| Chloroquine pholcodine meth MDA MDMA pseudoephedrine ketamine totokaine fenazil imipramine Chlorprothixene thebaine morphine O6-monoacetylmorphine heroin haloperole diazepam quinine | 150-10000 90-5000 90-5000 90-5000 90-5000 90-5000 60-5000 200-10000 90-5000 90-5000 60-5000 60-5000 60-5000 60-5000 60-5000 90-5000 90-5000 60-5000 | Y＝0.1277X+0.0011 Y＝0.5834X-0.0086 Y＝0.3253X-0.0089 Y＝0.3072X+0.0159 Y＝0.3592X-0.0098 Y＝0.2393X+0.0045 Y＝0.5016X-0.0141 Y＝0.1642X-0.0087 Y＝0.4068X-0.0145 Y＝0.5823X-0.0103 Y＝0.3542X-0.0047 Y＝0.9484X-0.1460 Y＝0.8338X-0.0541 Y＝0.8035X+0.0097 Y＝0.5110X-0.0213 Y＝0.4552X-0.0119 Y＝1.1236X-0.0266 Y＝0.5543X+0.0156 | 0.99875 0.99950 0.99960 0.99910 0.99910 0.99940 0.99955 0.99915 0.99940 0.99940 0.99945 0.99920 0.99905 0.99965 0.99945 0.99945 0.99975 0.99975 | 40 25 25 30 30 25 20 80 30 30 20 20 20 20 20 25 30 20 | 60-5000 60-5000 60-5000 60-5000 60-5000 200-10000 60-5000 60-5000 60-5000 60-5000 60-5000 60-5000 60-5000 60-5000 90-5000 60-5000 | Y＝0.3660X+0.0039 Y＝0.3626X+0.0037 Y＝0.4171X-0.0067 Y＝0.2197X-0.0030 Y＝0.4932X+0.0281 Y＝0.1473X+0.0037 Y＝0.4249X-0.0015 Y＝0.6045X+0.0290 Y＝0.4610X-0.0126 Y＝1.1088X+0.0521 Y＝1.0963X+0.0040 Y＝1.0851X+0.0386 Y＝0.6048X-0.0245 Y＝0.5906X+0.0045 Y＝1.0372X-0.0170 Y＝0.5512X-0.0052 | 0.99975 0.99970 0.99960 0.99940 0.99975 0.99920 0.99995 0.99940 0.99970 0.99935 0.99975 0.99965 0.99965 0.99985 0.99945 0.99955 | × × 20 20 20 20 20 80 20 20 20 15 25 15 20 20 30 20 |
| Clozapine procaine pethidine lidocaine hyoscine methadone Bupivacaine codeine O3-monoacetylmorphine fentanyl coscopin strychnia Lepetan amphetamine phenylpropanolamine ephedrine doxepin atropine codeine midazolam papaverine diphenoxylate cocaine perphenazine | 90-5000 90-5000 90-5000 90-5000 90-5000 60-5000 90-5000 60-5000 90-5000 90-5000 30-2000 90-5000 90-5000 90-5000 90-5000 90-5000 60-5000 90-5000 60-5000 90-5000 90-5000 90-5000 90-5000 150-10000 | Y＝0.5337X-0.0502 Y＝0.1647X-0.0194 Y＝0.1692X-0.0020 Y＝0.4680X-0.0168 Y＝0.1929X+0.0027 Y＝0.5171X+0.0155 Y＝0.4084X-0.0030 Y＝0.6363X+0.0180 Y＝0.3552X+0.0132 Y＝0.2491X+0.015 Y＝1.1532X-0.0260 Y＝0.4004X-0.0105 Y＝0.2799X-0.0004 Y＝0.2576X+0.0003 Y＝0.2085X+0.0374 Y＝0.2359X+0.0048 Y＝0.8853X-0.0331 Y＝0.2583X-0.0111 Y＝0.6089X-0.0039 Y＝0.2920X-0.0125 Y＝0.4272X-0.0120 Y＝1.1748X-0.0500 Y＝0.0781X-0.0043 Y＝0.0823X-0.0082 | 0.99945 0.99955 0.99985 0.99955 0.99990 0.99995 0.99990 0.99975 0.99965 0.99945 0.99975 0.99945 0.99980 0.99985 0.99810 0.99940 0.99995 0.99990 0.99990 0.99920 0.99950 0.99945 0.99965 0.99992 | 30 30 30 30 30 20 30 20 30 30 10 30 30 25 25 25 15 30 20 30 30 30 30 40 | 60-5000 150-10000 150-10000 60-5000 150-10000 90-5000 60-5000 60-5000 90-5000 30-20000 90-5000 90-5000 60-5000 90-5000 60-5000 90-5000 60-5000 90-5000 90-5000 90-5000 90-5000 150-10000 | Y＝0.8504X-0.0587 Y＝0.1530X-0.0328 Y＝0.1643X-0.0047 Y＝0.5569X-0.0030 Y＝0.2035X+0.0117 Y＝0.5179X+0.0265 Y＝0.5567X+0.0183 Y＝0.7679X+0.0305 Y＝0.2818X-0.0057 Y＝1.3069X-0.0339 Y＝0.6531X-0.0056 Y＝0.2578X-0.0159 Y＝0.3097X-0.0149 Y＝0.2032X+0.0059 Y＝1.2295X-0.0365 Y＝0.3369X+0.0448 Y＝0.7318X+0.0249 Y＝0.3120X+0.0124 Y＝0.5899X-0.0283 Y＝0.1873X-0.0233 Y＝0.1370X+0.0199 Y＝0.3888X-0.0782 | 0.99910 0.99885 0.99925 0.99975 0.99945 0.99945 0.99940 0.99920 0.99950 0.99935 0.99975 0.99950 0.99920 0.99970 0.99980 0.99960 0.99970 0.99975 0.99955 0.99990 0.99990 0.99990 | 20 40 40 20 40 30 20 15 × 30 10 30 30 20 × 30 20 30 30 30 30 30 30 40 |
| Fluphenazinum chlorpromazine strychnine Allylnoroxymorphone nordiazepam fluorine two dissolves triperazine anisodamine amobarbital quinalbarbitone amytal barbital phenobarbital | 150-10000 60-5000 30-2000 30-2000 30-2000 30-2000 150-10000 90-5000 90-10000 90-10000 90-10000 60-10000 60-10000 | Y＝0.1048X-0.0066 Y＝0.3493X-0.0104 Y＝0.7219X+0.0049 Y＝0.5056X-0.0127 Y＝0.7019X+0.0371 Y＝1.0040X+0.0031 Y＝0.1099X+0.0083 Y＝0.1948X-0.0030 Y＝0.5585X-0.0160 Y＝0.6340X+0.0101 Y＝0.8318X+0.0245 Y＝1.0446X-0.0303 Y＝1.5549X+0.0888 | 0.99960 0.99975 0.99995 0.99975 0.99935 0.99995 0.99975 0.99945 0.99970 0.99985 0.99990 0.99915 0.99960 | 40 20 5 5 5 5 40 30 30 30 30 20 20 | 150-10000 60-10000 30-20000 30-20000 30-20000 30-20000 150-10000 90-5000 800-25000 800-25000 800-25000 800-25000 800-25000 | Y＝0.2519X-0.0326 Y＝0.3620X+0.0178 Y＝0.9025X+0.1369 Y＝0.6308X+0.0377 Y＝1.0777X+0.1525 Y＝1.1038X+0.0983 Y＝0.5599X+0.0283 Y＝0.2342X+0.0100 Y＝0.1540X-0.0436 Y＝0.1867X-0.0013 Y＝0.2007X+0.0202 Y＝0.1928X+0.0989 Y＝0.4012X+0.1178 | 0.99965 0.99985 0.99915 0.99960 0.99905 0.99985 0.99975 0.99950 0.99980 1.00000 0.99995 0.99925 0.99955 | 40 20 8 8 8 8 40 30 100 100 100 200 50 |
3.4 absolute recovery
The absolute recovery of medicine poisonous substance sees Table 3.
The absolute recovery of table 3 medicine poisonous substance in urine and blood
| Medicine name | Drug usine level (ng/ml) | Average absolute recovery % in the urine | RSD (％) | Blood concentration (ng/ml) | Average absolute recovery % in the blood | RSD (％) |
| Chloroquine pholcodine meth MDA MDMA pseudoephedrine ketamine totokaine | 400.0 2000.0 5000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 400.0 2000.0 | 61.41 54.09 49.39 84.63 95.78 100.81 93.65 90.66 95.84 96.98 94.72 91.87 90.61 94.15 96.63 85.54 85.20 84.07 93.70 88.53 92.37 83.49 93.93 | 11.02 8.83 2.78 2.70 3.22 0.90 2.93 8.30 | 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 400.0 2000.0 | 94.35 98.61 92.51 94.35 93.61 93.04 89.27 94.46 92.16 74.33 67.77 64.29 95.03 96.63 104.45 70.33 68.87 | 3.28 0.69 2.83 7.40 5.10 3.18 |
| Fenazil imipramine Chlorprothixene thebaine morphine O6-monoacetylmorphine heroin haloperole diazepam quinine | 5000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 | 98.37 75.80 88.00 90.66 79.71 89.65 94.26 70.33 62.62 79.00 84.24 90.11 96.96 95.23 91.86 94.15 86.68 96.08 98.81 88.03 95.03 99.96 81.51 83.19 89.55 78.67 82.21 89.78 96.68 88.04 89.54 | 9.34 8.46 11.59 7.03 1.83 6.77 6.38 5.00 6.79 5.04 | 5000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 | 73.29 94.32 94.08 98.35 99.83 93.66 91.66 90.39 79.63 83.62 85.69 81.34 83.88 58.53 56.74 61.64 83.46 79.59 82.39 95.56 94.75 92.76 81.28 76.28 80.60 81.82 73.34 73.22 75.69 72.42 78.33 | 2.51 4.47 6.43 2.60 4.20 2.43 1.52 3.41 6.47 3.91 |
| Clozapine procaine pethidine lidocaine hyoscine methadone Bupivacaine codeine O3-monoacetylmorphine fentanyl | 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.00 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 | 77.29 73.88 62.12 71.73 82.79 87.27 96.16 89.82 92.03 100.47 85.54 93.58 95.40 82.59 92.88 94.45 77.55 93.40 93.15 79.98 84.47 94.01 79.72 82.30 98.80 90.57 92.58 99.02 87.54 93.50 | 11.18 9.92 3.47 8.01 7.51 10.70 7.79 8.92 4.56 6.15 | 200.0 1000.0 2000.0 400.0 2000.0 5000.0 400.0 2000.0 5000.0 200.0 1000.0 2000.0 400.0 2000.0 5000.00 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 | 63.86 61.57 72.71 57.39 53.46 54.85 66.79 59.59 66.63 68.84 69.81 78.92 78.16 76.23 89.20 62.61 73.30 71.64 92.96 99.51 94.92 76.20 68.88 76.57 63.65 65.10 74.93 | 8.90 3.60 6.39 7.66 8.61 8.31 3.51 5.86 9.03 |
| Coscopin strychnia Lepetan amphetamine phenylpropanolamine ephedrine doxepin atropine codeine midazolam | 100.0 500.0 1000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 | 93.60 97.06 101.30 82.56 86.21 85.75 98.52 84.98 88.78 84.73 88.46 86.05 59.89 65.99 69.72 93.11 91.80 97.80 82.02 78.88 94.51 102.86 86.02 101.91 100.80 93.34 96.10 86.46 80.46 89.57 | 3.96 2.34 7.69 2.18 7.61 3.34 9.70 9.76 3.90 5.45 | 100.0 500.0 1000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 | 77.08 71.91 83.51 87.88 74.78 84.45 65.54 67.81 61.22 77.48 70.44 79.48 69.32 68.65 79.81 77.12 83.12 86.70 85.01 100.91 99.12 84.31 91.93 100.42 70.09 73.46 77.56 | 7.49 8.24 5.16 6.25 8.62 5.88 9.16 8.73 5.07 |
| Papaverine diphenoxylate cocaine perphenazine fluphenazinum chlorpromazine strychnine Allylnoroxymorphone nordiazepam Flurazepam | 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 400.0 2000.0 5000.0 400.0 2000.0 5000.0 200.0 1000.0 2000.0 100.0 500.0 1000.0 100.0 500.0 1000.0 100.0 500.0 1000.0 100.0 500.0 1000.0 | 85.86 81.90 93.08 74.55 74.09 75.67 83.90 80.20 83.20 78.81 75.11 68.83 78.47 73.11 73.79 58.32 63.19 54.52 85.51 95.33 92.03 84.63 81.84 70.50 84.48 81.09 79.47 90.37 84.59 88.24 | 6.52 1.07 2.00 6.79 2.91 7.41 6.97 9.47 3.13 3.33 | 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 400.0 2000.0 5000.0 400.0 2000.0 5000.0 200.0 1000.0 2000.0 100.0 500.0 1000.0 100.0 500.0 1000.0 100.0 500.0 1000.0 100.0 500.0 1000.0 | 87.44 94.53 100.51 94.35 97.66 93.78 88.34 88.09 80.52 78.81 65.11 68.23 77.54 67.43 79.58 75.27 67.72 64.89 88.88 96.92 88.48 80.22 87.47 72.48 93.85 89.43 86.96 88.47 79.97 74.89 | 6.94 2.19 5.19 10.15 8.68 8.93 6.97 9.35 3.87 8.46 |
| Triperazine anisodamine doxapram (interior mark) amobarbital quinalbarbitone amytal barbital phenobarbital butalbital (interior mark) | 400.0 2000.0 5000.0 200.0 1000.0 2000.0 1250.0 150.0 1000.0 5000.0 150.0 1000.0 5000.0 150.0 1000.0 5000.0 150.0 1000.0 5000.0 150.0 1000.0 5000.0 4000.0 | 86.99 84.41 79.55 93.25 85.13 91.22 95.17 80.95 76.47 91.98 78.60 78.30 91.93 74.26 77.37 91.50 76.20 67.96 75.52 88.35 85.39 99.03 77.45 | 3.77 4.70 2.21 9.60 9.38 11.33 6.24 7.88 5.01 | 400.0 2000.0 5000.0 200.0 1000.0 2000.0 1000.0 1000.0 5000.0 20000.0 1000.0 5000.0 20000.0 1000.0 5000.0 20000.0 1000.0 5000.0 20000.0 1000.0 5000.0 20000.0 4000.0 | 80.25 85.33 79.16 75.16 80.33 82.79 94.42 94.82 89.48 85.19 97.20 91.58 86.78 92.31 92.39 91.49 95.16 96.19 61.26 62.73 69.10 91.14 92.34 99.48 85.52 | 4.03 4.93 3.20 6.57 3.54 2.62 6.46 4.78 3.08 |
3.5 relative recovery and precision
The relative recovery and the precision of each medicine poisonous substance see Table 4.
Relative recovery and the precision of table 4 medicine poisonous substance in urine and in the blood
| Medicine name | Drug usine level (ng/ml) | Average recovery rate % in the urine | Precision in the urine (%) | Blood concentration (ng/ml) | Average recovery rate % in the blood | Precision in the blood (%) | ||||
| Add concentration | Detectable concentration | In it | Between it | Add concentration | Detectable concentration | In it | Between it | |||
| Chloroquine pholcodine meth MDA MDMA pseudoephedrine | 400.0 2000.0 5000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 | 389.84 2104.40 4944.50 180.73 1010.38 2103.57 198.30 1026.47 2026.22 180.23 937.44 2056.46 198.86 1038.24 2024.63 187.74 | 97.46 105.22 98.89 90.36 101.03 105.17 99.15 102.64 99.43 90.11 93.74 102.82 99.43 103.82 101.23 93.87 | 7.38 5.33 1.55 3.33 3.18 2.24 1.73 2.42 0.38 6.48 5.20 3.98 0.21 0.24 0.58 2.31 | 5.69 3.33 5.47 2.55 3.17 4.33 2.44 1.36 4.95 9.38 4.20 5.03 2.68 1.83 4.66 3.35 | 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 | 194.26 996.44 2108.63 187.69 1022.41 1990.21 204.59 948.24 1963.43 197.25 | 97.13 99.64 105.43 93.84 102.24 99.51 102.30 94.82 98.17 98.63 | 2.54 3.30 3.93 3.07 4.33 1.98 5.90 1.89 8.50 6.37 | 6.99 1.95 2.73 4.11 5.72 2.73 7.75 7.59 6.82 10.17 |
| Ketamine totokaine fenazil imipramine Chlorprothixene thebaine morphine O6-monoacetylmorphine | 1000.0 2000.0 200.0 1000.0 2000.0 400.0 2000.0 5000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 | 1012.04 1969.16 183.54 1000.73 1963.67 391.28 2150.00 5108.50 191.76 1036.47 1966.91 186.40 951.26 2015.10 191.24 1066.55 2011.91 190.20 977.70 1981.81 203.82 1048.13 2039.61 209.54 | 101.20 98.45 91.77 100.73 98.18 97.82 105.75 102.17 95.88 103.64 98.34 93.20 95.12 100.75 95.62 106.65 100.59 95.10 97.77 99.09 101.91 104.81 101.98 104.77 | 4.57 5.22 1.07 0.69 2.14 4.13 1.28 2.71 3.24 1.81 1.68 0.68 1.12 0.75 7.97 2.06 4.56 1.82 1.77 0.69 5.81 2.47 1.40 3.81 | 3.41 4.46 1.47 1.51 4.08 2.72 3.12 4.15 5.87 1.98 3.90 1.04 2.90 3.87 6.93 3.30 6.33 6.94 1.38 4.41 6.69 1.37 4.29 3.92 | 1000.0 2000.0 200.0 1000.0 2000.0 400.0 2000.0 5000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 | 1001.65 2075.94 191.91 1045.85 2116.13 410.32 1995.65 5067.77 210.81 966.28 2059.88 194.90 984.15 2004.00 190.03 1035.01 1970.73 194.06 1051.12 2120.90 203.11 1040.03 2063.90 200.72 | 100.16 103.80 96.00 104.58 105.81 102.58 99.78 101.38 105.40 96.63 102.99 97.45 98.42 100.20 95.01 103.50 98.54 97.03 105.11 106.05 101.56 104.03 103.20 100.36 | 5.21 5.71 8.88 2.68 2.29 6.32 5.96 4.95 2.00 5.06 3.72 7.77 7.87 12.50 1.78 2.81 12.54 6.85 4.96 2.41 2.54 3.31 2.55 3.98 | 0.36 4.70 0.64 1.13 2.68 7.32 3.42 4.59 4.07 10.31 9.53 7.26 4.74 9.28 6.86 2.60 5.48 2.60 1.95 3.48 10.67 6.26 10.52 6.71 |
| Heroin haloperole diazepam quinine Clozapine procaine pethidine lidocaine | 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 | 1017.82 2015.43 198.50 989.38 2002.06 200.70 997.45 2010.96 189.60 1019.50 1995.98 187.91 978.44 2041.17 213.55 943.25 1924.58 210.83 951.01 1976.06 180.41 953.72 1934.66 212.81 | 101.78 100.77 99.25 98.93 100.10 100.35 99.74 100.54 94.80 101.95 99.79 93.95 97.84 102.05 106.77 94.32 96.22 105.41 95.10 98.80 90.20 95.37 96.73 106.40 | 2.12 0.96 1.54 0.09 3.00 4.22 1.19 1.08 3.76 1.55 2.49 5.24 7.54 1.78 3.05 2.94 3.48 7.75 6.25 4.05 5.29 4.56 5.38 2.29 | 2.74 3.32 0.90 2.87 5.05 7.55 3.35 5.10 1.97 1.58 2.92 5.67 4.91 5.25 7.25 4.77 5.23 11.68 7.33 7.50 9.40 7.40 5.26 5.78 | 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 400.0 2000.0 5000.0 400.0 2000.0 5000.0 200.0 | 1012.74 2085.94 189.80 958.34 1915.81 191.58 992.28 2075.53 210.36 1047.37 2115.91 195.24 1000.80 2054.93 200.97 947.53 2001.30 426.16 1912.60 5053.50 386.20 2014.00 5167.00 190.26 | 101.27 104.30 94.90 95.83 95.79 95.79 99.23 103.78 105.18 104.74 105.80 97.62 100.80 102.75 100.49 94.75 100.07 106.54 95.63 101.07 96.55 100.70 103.34 95.12 | 1.28 1.11 6.07 4.08 9.93 8.84 2.08 4.54 2.57 0.52 4.89 1.31 3.66 6.56 2.30 1.60 3.89 9.63 9.46 2.53 7.84 5.36 1.65 5.65 | 3.70 2.88 8.02 4.63 8.73 5.11 4.88 6.44 8.98 3.20 7.88 2.27 9.95 3.77 3.01 6.38 7.33 9.06 9.60 7.27 7.29 3.36 4.22 6.91 |
| Hyoscine methadone Bupivacaine codeine O3-monoacetylmorphine fentanyl coscopin strychnia | 1000.0 2000.0 200.0 1000.02000 .0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 100.0 500.0 1000.0 200.0 | 937.96 1914.96 190.13 1010.46 2031.45 197.77 986.42 2009.28 193.37 984.20 2027.71 195.72 978.72 2043.43 186.99 1010.93 2014.96 212.93 1076.72 2037.25 106.33 503.90 1018.60 215.96 | 93.79 95.73 95.06 101.04 101.57 98.88 98.64 100.46 96.68 98.42 101.38 97.71 97.87 102.17 93.49 101.09 100.74 106.46 107.67 101.86 103.66 100.78 101.86 107.98 | 2.96 5.89 3.66 4.51 3.42 5.36 4.73 5.44 4.01 4.53 7.51 5.91 5.96 4.27 4.25 4.14 5.06 7.01 7.84 5.57 5.78 4.26 2.23 6.08 | 1.43 3.84 6.38 9.87 8.38 9.10 5.11 3.81 8.93 7.93 7.50 11.59 7.26 7.91 6.88 2.77 5.98 8.80 5.80 5.31 7.70 1.52 3.33 4.95 | 1000.0 2000.0 400.0 2000.0 5000.00 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 100.0 500.0 1000.0 200.0 | 1021.30 2098.98 389.52 2106.00 5156.00 193.24 1042.02 2100.58 190.42 1042.13 1978.54 190.02 1054.10 2104.28 188.24 1028.09 2101.50 95.48 488.05 994.00 189.01 | 102.13 104.95 97.38 105.30 103.12 96.62 104.20 105.03 95.21 104.21 98.93 95.01 105.41 105.21 94.12 102.81 105.07 95.48 97.61 99.40 94.50 | 9.32 3.34 6.49 2.49 8.26 5.01 6.11 5.02 8.71 7.95 0.20 1.96 6.44 3.09 4.13 5.29 2.19 6.64 3.09 9.59 5.59 | 5.18 3.40 6.76 4.15 4.34 3.36 2.05 7.16 3.09 10.14 4.36 4.19 5.10 5.62 2.67 0.73 10.16 9.59 5.75 7.67 5.17 |
| Lepetan amphetamine phenylpropanolamine ephedrine doxepin atropine codeine midazolam | 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 | 980.36 2130.79 208.37 950.21 1929.50 186.84 1019.64 2096.32 185.56 998.76 2017.80 194.35 972.27 2028.47 198.71 987.15 2005.57 189.95 985.59 2005.81 201.19 990.45 2045.76 207.79 | 98.03 106.53 104.19 95.02 96.47 93.42 101.96 104.81 92.78 99.87 100.89 97.17 97.22 101.42 99.97 98.71 100.27 94.97 98.55 100.29 100.59 99.04 102.28 103.89 | 2.11 2.13 11.69 6.84 8.09 3.08 5.75 4.57 9.26 5.57 4.18 2.35 1.88 2.26 2.75 7.31 4.08 7.05 7.66 0.98 2.20 5.56 1.67 5.56 | 2.72 1.51 6.88 4.53 9.88 0.75 2.46 4.74 5.66 3.06 2.09 3.14 3.26 5.00 3.21 5.78 6.25 7.43 5.29 2.03 8.09 1.54 3.90 5.32 | 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 | 1061.56 2052.05 192.93 918.71 2048.37 206.44 975.86 1975.03 206.03 934.10 2069.01 212.33 1016.26 1929.79 207.24 1056.93 1994.69 193.12 1053.70 2045.32 195.50 | 106.16 102.60 96.46 91.87 102.42 103.22 97.58 98.75 103.01 93.41 103.45 106.16 101.62 96.48 103.62 105.69 99.73 96.56 105.37 102.26 97.75 | 8.25 2.21 6.01 11.96 4.64 3.40 1.80 3.19 8.61 3.59 4.49 5.08 8.58 11.87 8.58 6.09 4.41 4.23 5.29 1.42 6.15 | 1.33 8.04 9.35 6.43 9.41 10.94 5.90 9.14 2.47 8.33 10.94 7.38 3.72 4.14 12.82 11.79 3.95 12.59 7.18 7.18 6.95 |
| Papaverine diphenoxylate cocaine perphenazine fluphenazinum chlorpromazine strychnine Allylnoroxymorphone | 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 400.0 2000.0 5000.0 400.0 2000.0 5000.0 200.0 1000.0 2000.0 100.0 500.0 1000.0 100.0 | 971.99 1970.00 194.99 1029.34 1980.37 209.64 969.29 2011.53 215.57 973.07 2012.50 432.26 1903.26 5051.12 432.64 1942.54 5034.57 184.29 1028.65 1987.67 102.56 495.40 1002.00 93.37 | 97.19 98.50 97.49 102.92 99.01 104.82 96.92 100.57 107.78 97.30 100.62 108.14 95.16 101.02 108.16 97.12 100.69 92.14 102.86 99.38 102.56 99.08 100.20 93.37 | 2.03 4.47 7.04 2.36 6.77 6.77 6.40 2.71 7.38 1.19 3.30 5.68 5.77 8.38 3.68 7.38 4.68 10.38 5.73 5.28 10.22 4.88 7.31 5.10 | 2.41 2.95 5.06 8.41 1.66 9.47 9.61 4.87 5.47 3.34 0.99 9.59 7.62 8.61 3.88 5.34 1.56 9.34 3.35 8.47 5.31 2.24 2.57 5.10 | 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 200.0 1000.0 2000.0 400.0 2000.0 5000.0 400.0 2000.0 5000.0 200.0 1000.0 2000.0 100.0 500.0 1000.0 100.0 | 1074.24 2037.95 206.11 1012.16 1892.33 203.23 955.41 2062.01 221.19 1048.40 2028.93 416.56 1970.20 5016.50 429.68 1946.20 5029.00 190.15 1017.69 1992.02 97.07 521.70 990.30 91.59 | 107.42 101.89 103.05 101.21 94.61 101.62 95.54 103.10 110.05 104.84 101.44 104.14 98.51 100.33 107.42 97.31 100.58 95.07 101.76 99.60 97.07 104.34 99.03 91.59 | 1.63 9.12 1.14 4.86 3.53 2.40 1.98 5.01 7.67 9.66 3.91 5.35 5.86 8.13 4.68 7.18 5.06 0.43 3.66 2.49 2.60 4.87 10.55 0.17 | 3.37 4.85 3.62 9.57 5.04 6.23 5.40 6.22 3.39 5.65 6.33 10.59 7.42 8.01 6.44 6.24 1.02 5.52 4.40 7.53 1.82 1.38 2.94 4.84 |
| Nordiazepam Flurazepam triperazine anisodamine amobarbital quinalbarbitone amytal | 500.0 1000.0 100.0 500.0 1000.0 100.0 500.0 1000.0 400.0 2000.0 5000.0 200.0 1000.0 2000.0 150.0 1000.0 5000.0 150.0 1000.0 5000.0 150.0 1000.0 5000.0 | 511.80 994.70 94.68 518.45 991.80 101.60 479.25 1009.20 379.88 2015.55 5005.99 195.88 998.36 2044.36 165.34 942.81 4830.44 141.89 940.68 5004.82 149.82 960.71 4988.79 | 102.36 99.47 94.68 103.69 99.18 101.60 95.85 100.92 94.97 100.77 100.11 97.94 99.83 102.20 110.23 94.28 96.60 94.59 94.06 100.09 99.88 96.07 99.77 | 0.99 3.00 5.32 1.13 8.95 6.85 1.81 9.01 6.48 3.85 2.78 4.69 6.33 2.67 7.38 1.73 4.23 9.05 5.46 4.24 3.41 1.07 1.94 | 2.44 7.36 5.31 1.52 2.96 9.35 3.48 7.57 8.22 4.68 1.67 3.77 9.18 1.72 6.97 5.62 4.62 9.73 3.99 2.09 10.3 5 4.17 2.41 | 500.0 1000.0 100.0 500.0 1000.0 100.0 500.0 1000.0 400.0 2000.0 5000.0 200.0 1000.0 2000.0 1000.0 5000.0 20000.0 1000.0 5000.0 20000.0 1000.0 5000.0 20000.0 | 515.10 993.20 91.82 522.35 990.00 104.77 491.35 1003.80 386.88 2006.40 5043.00 191.88 983.57 2015.86 1023.79 4809.92 20117.19 1068.52 4758.76 19992.89 1058.05 4698.77 20036.25 | 103.02 99.32 91.82 104.47 99.00 104.77 98.27 100.38 96.72 100.32 100.86 95.94 98.35 100.79 102.37 96.19 100.58 106.85 95.17 99.96 105.80 93.97 100.18 | 0.32 3.51 1.14 5.59 7.82 5.95 1.44 5.42 7.38 4.66 2.68 4.36 0.78 6..59 7.22 8.88 8.16 3.39 7.02 11.60 6.86 9.13 11.32 | 3.00 6.70 9.59 3.86 1.93 3.57 9.73 4.09 6.22 5.89 2.69 3.55 7.25 1.49 7.88 8.82 2.46 6.81 6.81 3.04 6.05 3.69 1.42 |
| The barbital phenobarbital | 150.0 1000.0 5000.0 150.0 1000.0 5000.0 | 160.93 1005.17 5034.48 140.91 1047.44 5190.80 | 107.29 100.51 100.68 93.94 104.74 103.81 | 9.04 8.55 13.09 2.90 0.87 0.78 | 10.3 5 7.49 5.41 3.51 1.96 1.56 | 1000.0 5000.0 20000.0 1000.0 5000.0 20000.0 | 1013.55 4914.02 19976.97 992.75 4766.66 20048.51 | 101.35 98.28 99.88 99.27 95.33 100.24 | 7.78 8.76 3.74 11.91 4.03 6.79 | 11.43 3.80 3.54 5.95 1.35 1.08 |
Drugs analysis in person's urine sample that embodiment 2 takes the head-shaking pill
The urine sample source: drug testing center, Shanghai City, outward appearance is limpid.
Blank urine sample and other medicine, reagent and used instrument material are with embodiment 1.
Working curve: with embodiment 1.
Sample preparation: with embodiment 1.
Instrument condition is with embodiment 1.
Detect in the urine sample of taking head-shaking pill suspicion person and contain MDA, concentration is 4120ngmL
-1Chromatogram is seen Fig. 6.
Drugs analysis in embodiment 3 drug addict's urine samples
The urine sample source: drug testing center, Shanghai City, outward appearance is limpid.
Blank urine sample and other medicine, reagent and used instrument material are with embodiment 1.
Working curve: with embodiment 1.
Sample preparation: with embodiment 1.
Instrument condition is with embodiment 1.
The result shows, MDMA content surpasses the working curve scope in the urine sample, for obtaining correct quantitative data, measures once more after getting 5 times of this urine sample dilute with waters, detects meth, MDMA and ketamine in drug addict's urine sample, and concentration is respectively 2917ngmL
-1, 8512ngmL
-1And 887ngmL
-1Chromatogram is seen Fig. 7.
Drugs analysis in embodiment 4 drug addict's urine samples
The urine sample source: drug testing center, Shanghai City, outward appearance is limpid.
Blank urine sample and other medicine, reagent and used instrument material are with embodiment 1.
Working curve: with embodiment 1.
Sample preparation: with embodiment 1.
Instrument condition is with embodiment 1.
Detect the morphine composition in drug addict's urine sample, concentration is 794.8ngmL
-1Chromatogram is seen Fig. 8.
The urine sample source: drug testing center, Shanghai City, outward appearance is limpid.
Blank urine sample and other medicine, reagent and used instrument material are with embodiment 1.
Working curve: with embodiment 1.
Sample preparation: with embodiment 1.
Instrument condition is with embodiment 1.
Detect the lidocaine composition in the poisoning patient whole blood, concentration is 3372ngmL
-1, chromatogram is seen Fig. 9.
The urine sample source: drug testing center, Shanghai City, outward appearance is limpid.
Blank urine sample and other medicine, reagent and used instrument material are with embodiment 1.
Working curve: with embodiment 1.
Sample preparation: with embodiment 1.
Instrument condition is with embodiment 1.
Detect the doxepin composition in the poisoning patient whole blood, concentration is 1930ngmL
-1, chromatogram is seen Figure 10.
The urine sample source: drug testing center, Shanghai City, outward appearance is limpid.
Empty from urine sample and other medicine, reagent and used instrument material with embodiment 1.
Working curve: with embodiment 1.
Sample preparation: with embodiment 1.
Instrument condition is with embodiment 1.
Detect phenobarbital in injured party's urine, concentration is 6358.08ngmL
-1, chromatogram is seen Figure 11.
Claims (6)
1, a kind of high performance capillary electrophoresis method that detects blood, urine Chinese medicine poisonous substance simultaneously comprises the steps:
A, sample preparation: adopt Solid-Phase Extraction, stationary phase is C
18, C
8, bonding phase silica gel, polymkeric substance or macroporous resin adsorption materials such as CN or phenyl, acid or alkaline medicine poisonous substance is respectively with containing acid or contain alkali and the aqueous solution drip washing of organic solvent, and uses the organic solvent wash-out respectively, the intact back of its neutral and alkali medicine poisonous substance wash-out adds acid;
B, capillary electrophoresis separation: inorganic salts damping fluid and organic solvent are formed running buffer, wherein the inorganic salts damping fluid is phosphate buffer or borate buffer solution, and organic solvent is methyl alcohol or acetonitrile, quartz capillary column, pressure sample introduction, separation voltage are 5-20kv; Column temperature is 15-30 ℃;
C, ultraviolet detection.
2, capillary electrophoresis method according to claim 1, it is characterized in that containing sour leacheate is acetate, hydrochloric acid or phosphoric acid, containing the alkali leacheate is ammoniacal liquor, NaOH or sodium carbonate, the organic solvent leacheate is methyl alcohol, ethanol or acetonitrile.
3, capillary electrophoresis method according to claim 1 is characterized in that the sample of selecting for use is a whole blood, adds acid when handling whole blood, as phosphoric acid, sulfuric acid or oxalic acid.
4, capillary electrophoresis method according to claim 1 is characterized in that after the Solid-Phase Extraction drip washing the solid-phase extraction column centrifuge dripping.
5, capillary electrophoresis method according to claim 1 is characterized in that the damping fluid of capillary electrophoresis analysis alkalescence poisonous substance is phosphate and methyl alcohol or acetonitrile; The damping fluid of analyzing acid poisonous substance is borate and methyl alcohol or acetonitrile.
6, capillary electrophoresis method according to claim 1 is characterized in that with butalbital or doxapram respectively as the interior mark of acid or alkaline medicine poisonous substance.
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| CN103344710A (en) * | 2013-06-05 | 2013-10-09 | 公安部物证鉴定中心 | Method for detecting diphenoxylate in biological sample by liquid chromatography-tandem mass spectrometry for criminal investigation |
| CN105277606A (en) * | 2014-07-08 | 2016-01-27 | 山东绿叶制药有限公司 | Determination method for exenatide related substance |
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| CN112362765A (en) * | 2020-10-13 | 2021-02-12 | 长沙都正生物科技股份有限公司 | Doxepin and metabolite N-nor-doxepin solid-phase extraction and detection method and kit thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103344710A (en) * | 2013-06-05 | 2013-10-09 | 公安部物证鉴定中心 | Method for detecting diphenoxylate in biological sample by liquid chromatography-tandem mass spectrometry for criminal investigation |
| CN103344710B (en) * | 2013-06-05 | 2015-08-05 | 公安部物证鉴定中心 | Use liquid chromatography-tandem mass spectrometry for criminal investigation object detects the method for diphenoxylate in biological sample |
| CN105277606A (en) * | 2014-07-08 | 2016-01-27 | 山东绿叶制药有限公司 | Determination method for exenatide related substance |
| CN106770804A (en) * | 2017-02-28 | 2017-05-31 | 云南农业大学 | The detection method of terramycin content in tobacco seedling |
| CN109406608A (en) * | 2018-12-20 | 2019-03-01 | 兰州大学 | The method and application of Dynamic coating are carried out to capillary using humoral sample solution to be measured |
| CN110988093A (en) * | 2019-12-24 | 2020-04-10 | 青岛大学附属医院 | Method for detecting content of high-salt blood cardiovascular drug |
| CN110988093B (en) * | 2019-12-24 | 2022-03-04 | 青岛大学附属医院 | Method for detecting content of high-salt blood cardiovascular drug |
| CN111537628A (en) * | 2020-04-15 | 2020-08-14 | 无锡微色谱生物科技有限公司 | DPX-GC-MS detection method for 2-chlorodiazepam and 4-chlorodiazepam in urine |
| CN111537628B (en) * | 2020-04-15 | 2022-04-26 | 无锡微色谱生物科技有限公司 | DPX-GC-MS detection method for 2-chlorodiazepam and 4-chlorodiazepam in urine |
| CN112362765A (en) * | 2020-10-13 | 2021-02-12 | 长沙都正生物科技股份有限公司 | Doxepin and metabolite N-nor-doxepin solid-phase extraction and detection method and kit thereof |
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