CN105572241A - Method for assaying amphetamines, ketamine, pethidine and methadone in blood and urine - Google Patents
Method for assaying amphetamines, ketamine, pethidine and methadone in blood and urine Download PDFInfo
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Abstract
The invention belongs to the technical field of analytical chemistry, and relates to a method for rapidly assaying four amphetamines (amphetamine, methamphetamine, methylene-dioxy-amphetamine and methylene-dioxy-methamphetamine), ketamine, pethidine and methadone in blood and urine. The method is high in sensitivity and specificity and wide in linear range, can be used for qualitatively and quantitatively assaying analytes of unknown concentrations in the blood and the urine, and is simple and rapid to operate; according to the method, processes of extracting, and drying by evaporating are not required, and characteristics that a judicial expertise task is urgent and has a high requirement on assaying time can be met; an assaying system, provided by the invention, provides a new technical platform for drug assaying, and is easy to popularize and apply.
Description
Technical field
The invention belongs to analytical chemistry field, be specifically related to a kind of method measuring amphetamine, ketamine, pethidine and methadone in blood and urine.This method can the compound such as 4 kinds of amphetamines (amphetamine, crystal methamphetamine, MDA, methylene benzylene chloride propylamine) ketamine, pethidine and methadones in easy Fast Measurement blood and urine, is particularly useful for judicial expertise field.
Background technology
According to data, 4 kinds of amphetamine compound (amphetamine (amphetamine are comprised at present by the drugs extensively abused, AMP), crystal methamphetamine (methamphetamine, MAMP), MDA (methylenedioxyamphetamine, MDA), methylene benzylene chloride propylamine (methylenedioxymethamphetamine, and ketamine and pethidine MDMA).
Research display, its toxicity of AMP and MAMP mainly act as master with central nervous system stimulant; MDA, MDMA have excitement and hallucinogenic action concurrently, are the principal ingredients being called as dancing outreach drugs.Ketamine, also referred to as " KET ", has hallucinogenic action, and Long-Time Service or excessive use can cause permanent damage to brain; Pethidine has another name called meperidine, and be clinical conventional analgestic, Long-Time Service can produce dependence, is listed in the drugs of strict supervision in China; Methadone because of its pharmacological action similar to morphine, withrawal symptom is comparatively light, for the opium drugs such as heroin rely on the choice drug carrying out alternative successive subtraction method drug addiction treatment, therefore in the qualification of case of being involved in drug traffic, has higher recall rate.
Judicial expertise practice display, blood and urine are of paramount importance biological materials in drugs qualification; Wherein, in urine, the concentration of drugs is high, and therefore, urine is that sample is commonly used in drugs qualitative analysis; Blood is the sample that drugs quantitative test is commonly used, and the quantitative value of gained can be compared with the poisoning concentration of bibliographical information or lethasl concentration.
The disclosed method measuring amphetamine, ketamine, pethidine, methadone in blood and urine of prior art has euzymelinked immunosorbent assay (ELISA), GC-MS(gas chromatography-mass spectrography), Liquid Chromatography-Mass Spectrometry etc. usually.Practice display, described euzymelinked immunosorbent assay (ELISA) specificity is poor, be difficult to specification configuration analog, the false-positive situation of normal appearance, thus, can only as a kind of means of primary dcreening operation, need to adopt GC-MS(gas chromatography-mass spectrography) or Liquid Chromatography-Mass Spectrometry to confirm further, and biological sample is being carried out before GC-MS(gas chromatography-mass spectrography) or Liquid Chromatography-Mass Spectrometry analyze, all need to carry out Isolation and purification to sample, and this step relates to the process volatilized by extract, therefore normal generation also shows after deliberation, AMP and MAMP volatilizees fast along with volatilizing of extract, the reappearance of impact analysis and the linear of typical curve, analyte described in biological material is caused to be difficult to the defect of accurate quantitative analysis.Have researchist by acid adding or under using cryogenic conditions, sample volatilized or operate the volatilization to avoiding AMP and MAMP by derivatization, but the method adopted is loaded down with trivial details and consuming time, is still difficult to meet judicial expertise for drugs of abuse requirement fast.
Present inventor for current present situation, intend providing a kind of easy, fast and accurately can the method for 4 kinds of amphetamines (amphetamine, crystal methamphetamine, MDA, methylene benzylene chloride propylamine), ketamine, pethidine, methadone content in Simultaneously test blood and urine.
Summary of the invention
The object of the invention is the defect overcoming prior art, a kind of method measuring amphetamine, ketamine, pethidine and methadone in blood and urine is provided; Especially a kind of easy, fast and accurately can the method for 4 kinds of amphetamines (amphetamine, crystal methamphetamine, MDA, methylene benzylene chloride propylamine), ketamine, pethidine, methadone content in Simultaneously test blood and urine.This method can meet judicial expertise for drugs of abuse requirement fast.
Concrete, the inventive method adopts GC-MS(gas chromatography-mass spectrography) to carry out qualitative and quantitative analysis to 4 kinds of amphetamines, ketamine, pethidine, methadones in blood and urine.In this method, to a small amount of blood and urine (0.2-1mL) after basification, add a small amount of organic solvent (1-chlorobutane, 100-300 μ L) carry out liquid-liquid extraction, transfer upper layer of extraction liquid directly adopts GC-MS(gas chromatography-mass spectrography) to carry out measuring (sample size 2 μ L), can measure the content of analyte.
The pretreatment process of the inventive method sample is easy, quick, be easy to promote; The present invention adopts HP-5MS capillary gas chromatographic column and mass detector, to measure in blood and urine the content of 4 kinds of amphetamines, ketamine, pethidine, methadone, detection highly sensitive, accuracy good.
More specifically, the method for amphetamine, ketamine, pethidine and methadone in mensuration blood of the present invention and urine, it is characterized in that, extract directly adopts GC-MS(gas chromatography-mass spectrography) to measure, and comprises the steps:
(1) to blood or urine sample pre-service
Get blood or urine sample, add interior mark, add 10%NaOH solution and sample is adjusted to strong basicity, then add 1-chlorobutane, the centrifugal 5min of vortex mixed 2min, 10000rpm, transfer upper organic phase;
(2) concentration of 4 kinds of amphetamines, ketamine, pethidine and methadones in gas chromatography/mass spectrometry blood or urine sample is adopted; Chromatographic column is HP-5MS capillary column.
In the present invention, only need take a morsel blood or urine sample sample carry out pre-service, and blood or the urine sample sample of getting 0.2-1mL in embodiments of the invention carry out pre-service;
In the present invention, in blood or urine sample sample, add interior mark MAMP-D5, in blood or urine sample sample, in embodiments of the invention, add interior mark MAMP-D50.2-1 μ g, then add 10%NaOH solution sample is adjusted to strong basicity;
In the present invention, use 1-chlorobutane as Extraction solvent in blood and urine sample pretreatment operation, what do not relate to extract volatilizes process, 1-chlorobutane 100-300 μ L is added in embodiments of the invention, the centrifugal 5min of vortex mixed 2min, 10000rpm, transfer upper organic phase;
In the present invention, after adding 1-chlorobutane, what do not relate to extract volatilizes process, is detected by extract direct injected gas chromatograph-mass spectrometer (GCMS);
In the present invention, the chromatographic column of employing is HP-5MS capillary column (30m × 0.25mm × 0.25 μm), sample size 2 μ L.
The present invention has carried out qualitative and quantitative analysis to 4 kinds of amphetamines, ketamine, pethidine, methadones in blood and urine, and result accurately, reliably; Each compound test limit is 5ng/mL, and be quantitatively limited to 20ng/mL, the range of linearity 0.02 ~ 25 μ g/mL, linearly dependent coefficient r value is all greater than 0.99.For blood sample, extraction recovery is within the scope of 33.7-80.5%, and accuracy is within the scope of 87.1-113.9%, and the RSD value of withinrun precision is no more than 10.2%, and the RSD value of betweenrun precision is no more than 12.1%; For urine sample, extraction recovery is within the scope of 64.6-112.6%, and accuracy is within the scope of 85.1-108.4%, and the RSD value of withinrun precision is no more than 6.3%, and the RSD value of betweenrun precision is no more than 11.5%.
Table 1 is for detecting chromatographic retention and the mass spectral characteristic peak of object.
Table 1
The Measures compare of the inventive method and prior art has following clear superiority:
(1) compared with euzymelinked immunosorbent assay (ELISA), the inventive method highly sensitive, the detectability of each compound can reach 5ng/mL, and the detection of euzymelinked immunosorbent assay (ELISA) is limited to 300-1000ng/mL.And for the detection of drugs, way current in the world first carries out primary dcreening operation by euzymelinked immunosorbent assay (ELISA), confirm with GC-MS(gas chromatography-mass spectrography) or Liquid Chromatography-Mass Spectrometry, thus the sensitivity of the inventive method is enough to meet the needs of actual inspection case in judicial expertise work again.
(2) compared with the GC-MS(gas chromatography-mass spectrography) of prior art or Liquid Chromatography-Mass Spectrometry, the inventive method greatly simplifies the pre-treatment step of sample; The method of prior art all needs the process dried up by the extract of sample, longer (more than 30min) consuming time, and be difficult to avoid 2 kinds of important amphetamine materials (AMP and MAMP) to lose along with the volatilization of extract, carry out the reappearance of impact analysis and the linear of typical curve, cause these 2 kinds of materials in biological material to be difficult to accurate quantitative analysis; Though have researchist by acid adding or volatilize sample under using cryogenic conditions or operate the volatilization to avoiding AMP and MAMP by derivatization, these methods are loaded down with trivial details and consuming time, are difficult to meet judicial expertise for drugs of abuse requirement fast; The step of the inventive method sample pre-treatments avoids the process dried up, and does not need other sample handling procedure, ensure that the linear of typical curve, guarantees the accuracy of quantitative result; Simultaneously easy, quick (time for sample pretreatment is within 10min), the efficiency of drugs qualification can be improved significantly.
(3) the whole blood sample amount few (can be low to moderate 0.2mL, prior art is 0.95-2mL) of the inventive method use, can tackle the situation that in legal medical expert's case, sample amount is usually very limited.
(4) consumption of organic solvent few (100-300 μ L, prior art is 1.5-5mL) of the inventive method use, little to the healthy harm of operating personnel, more friendly to environment, can save analysis cost.
Accompanying drawing explanation
Fig. 1 is the standard colors spectrogram of 4 kinds of amphetamines, ketamine, pethidine, methadone,
Wherein, AMP (3.6min), MAMP (4.0min), MDA (5.8min), MDMA (6.1min), pethidine (7.2min), ketamine (7.7min) and methadone (8.8min) and internal standard compound MAMP-D5 (4.0min).
Embodiment
Embodiment 1
The chromatographic condition adopted:
Chromatographic column: HP-5MS elastic quartz capillary tube gas chromatographic column, 30m × 0.25mm × 0.25 μm
Column temperature: 100 DEG C of (1.5min)-25 DEG C/min-280 DEG C (15min)
The solvent delay time: 3min
Injection port/transmission line temperature: 250 DEG C/280 DEG C
Carrier gas: high-purity He, constant current 1mL/min
EI source electron energy: 70Ev
Scan mode: Salbutamol Selected Ion Monitoring (SIM)
Sample size: 2 μ L
Detect chromatographic retention and the mass spectral characteristic peak of object: as shown in table 1.
Sample preparation:
(1) extraction of blood sample
Get blood sample 0.2-1mL, add interior mark (MAMP-D5) 0.2-1 μ g, add 10%NaOH solution 0.05mL and mix, add 1-chlorobutane 100-300 μ L again, the centrifugal 5min of vortex mixed 2min, 10000rpm, transfer upper organic phase 50-100 μ L analyzes for GC-MS;
(2) extraction of urine sample
Get urine sample 0.2-1mL, add interior mark (MAMP-D5) 0.2-1 μ g, 10%NaOH solution is adopted to be adjusted to pH>11, add 1-chlorobutane 100-300 μ L again, vortex mixed 2min, the centrifugal 5min of 10000rpm, transfer upper organic phase 50-100 μ L analyzes for GC-MS;
Linear test:
Get hybrid standard series of working liquids, add blank whole blood and urine, vortex mixes, be made into the standard plasma containing drug and the urine that are respectively 0.02,0.05,0.1,0.5,1,5,10,25 μ g/ml containing testing concentration, operate by under " sample preparation " item, preparation standard curve, and prepare blank sample, record chromatogram simultaneously; Take testing concentration as horizontal ordinate, determinand and interior target peak area ratio are ordinate, carry out regressing calculation, drawing standard curve by weighting (W=1/x2) least square method;
Preci-sion and accuracy is tested:
Get the basic, normal, high Quality Control working fluid of hybrid standard, add blank whole blood and urine, vortex mixes, and is made into and is respectively 0.05 containing testing concentration, 1, the pastille whole blood of 20 μ g/mL and urine; Often criticize each concentration and prepare 5 parts, do 3 batches altogether; Operate by under " sample preparation " item; Calculate its measured concentration according to often criticizing equation of linear regression, calculate the accuracy of each concentration, batch interior and betweenrun precision, precision represents with relative standard deviation (RSD);
Recovery test:
Get basic, normal, high concentration hybrid standard Quality Control working fluid to be mixed with and to be respectively 0.05 containing testing concentration, 1, the pastille whole blood of 20 μ g/mL and each 5 parts of urine, operate by under " sample preparation " item, record sample and interior mark peak area AS1, AS2 and AIS1; (getting a collection of precision data to calculate) separately operates gained bare substrate liquid with blank whole blood or urine by under " sample preparation " item, add hybrid standard working fluid, the contrast solution of preparation 3 same concentrations, the parallel preparation of each concentration 3 parts, record sample and interior mark peak area computation of mean values AS3, AS4 and AIS2, calculate the recovery with AS1/AS3 × 100%, AS2/AS4 × 100% and AIS1/AIS2 × 100%.
Result shows, and the pretreatment process of the inventive method sample is easy, quick, and needs sample size few, and the consumption of organic solvent of use is few; Adopt HP-5MS capillary gas chromatographic column and mass detector, to measure in blood and urine the content of 4 kinds of amphetamines, ketamine, pethidine, methadone, detect easy, quick, highly sensitive, accuracy is good, can improve the efficiency of drugs qualification significantly.
Table 2 be in people's whole blood determinand batch in and betweenrun precision, accuracy and extraction recovery data.
Table 3 be in human urine determinand batch in and betweenrun precision, accuracy and extraction recovery data.
Table 2
Table 3
Claims (7)
1. measure the method for amphetamine, ketamine, pethidine and methadone in blood and urine, it is characterized in that, directly adopted by extract GC-MS(gas chromatography-mass spectrography) to measure, comprise the steps:
(1) to blood or urine sample pre-service
Get blood or urine sample, add interior mark, add 10%NaOH solution and described sample is adjusted to strong basicity, then add Extraction solvent, the centrifugal 5min of vortex mixed 2min, 10000rpm, transfer upper organic phase;
(2) concentration of 4 kinds of amphetamines, ketamine, pethidine and methadones in gas chromatography/mass spectrometry blood or urine sample is adopted; Chromatographic column is HP-5MS capillary column.
2., by method according to claim 1, it is characterized in that, described amphetamine compound is amphetamine, crystal methamphetamine, MDA and or/methylene benzylene chloride propylamine.
3., by method according to claim 1, it is characterized in that, described Extraction solvent is 1-chlorobutane.
4. by method according to claim 1, it is characterized in that, what do not relate to extract in described blood and urine sample pre-service volatilizes process, is detected by extract direct injected gas chromatograph-mass spectrometer (GCMS).
5., by method according to claim 1, it is characterized in that, described blood or urine sample sample are 0.2-1mL.
6., by method according to claim 1, it is characterized in that, in described blood or urine sample sample, add interior mark MAMP-D50.2-1 μ g.
7., by method according to claim 1, it is characterized in that, the condition of described chromatogram is:
Chromatographic column: HP-5MS capillary column, 30m × 0.25mm × 0.25 μm; Column temperature: 100 DEG C of 1.5min-25 DEG C/min-280 DEG C 15min; The solvent delay time: 3min; Injection port/transmission line temperature: 250 DEG C/280 DEG C; Carrier gas: high-purity He, constant current 1mL/min; EI source electron energy: 70Ev; Scan mode: Salbutamol Selected Ion Monitoring SIM.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106501414A (en) * | 2016-12-07 | 2017-03-15 | 公安部物证鉴定中心 | A kind of method that homogenizes of amphetamine tablet |
| CN106645487A (en) * | 2016-12-28 | 2017-05-10 | 上海微谱化工技术服务有限公司 | Detection and analysis method for methamphetamine in weight-reducing drug |
| CN107340347A (en) * | 2017-05-08 | 2017-11-10 | 公安部物证鉴定中心 | Method for preparing purified for the Sauteralgyl standard substance of forensic science illicit drugs inspection |
| CN109507354A (en) * | 2019-01-17 | 2019-03-22 | 浙江工业大学 | The method of Ketamine content in Flash evaporation gas chromatography mass spectrometric determination human hair |
| CN110823855A (en) * | 2019-12-19 | 2020-02-21 | 鄂尔多斯应用技术学院 | Method for rapidly detecting amphetamine drugs in human urine |
| WO2022151842A1 (en) * | 2021-01-14 | 2022-07-21 | 浙江海正药业股份有限公司 | Gas-phase chromatography detection method for dicyclohexylamine in favipiravir |
| CN115060815A (en) * | 2022-05-30 | 2022-09-16 | 广西大学 | Solid phase extraction-liquid chromatography-ion trap/time-of-flight mass spectrometry combined detection method for fluoroamidone metabolites in human urine |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100848132B1 (en) * | 2008-05-27 | 2008-07-25 | 대한민국 | Simultaneous determination of amphetamine-type stimulants and cannabinoids by gas chromatography |
| CN102128905A (en) * | 2010-12-10 | 2011-07-20 | 中国广州分析测试中心 | Method for quickly detecting drug |
| CN103808846A (en) * | 2014-02-20 | 2014-05-21 | 福建国际旅行卫生保健中心 | Series quadrupole-rod gas-chromatographic mass spectrometry detection method for 35 toxic medicaments in urine |
-
2014
- 2014-11-05 CN CN201410619166.1A patent/CN105572241B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100848132B1 (en) * | 2008-05-27 | 2008-07-25 | 대한민국 | Simultaneous determination of amphetamine-type stimulants and cannabinoids by gas chromatography |
| CN102128905A (en) * | 2010-12-10 | 2011-07-20 | 中国广州分析测试中心 | Method for quickly detecting drug |
| CN103808846A (en) * | 2014-02-20 | 2014-05-21 | 福建国际旅行卫生保健中心 | Series quadrupole-rod gas-chromatographic mass spectrometry detection method for 35 toxic medicaments in urine |
Non-Patent Citations (3)
| Title |
|---|
| 卓先义等: "尿中氯胺酮及其代谢物检测的研究", 《中国司法鉴定》 * |
| 孟品佳等: "生物样品中苯丙胺类毒品的小体积液相萃取及GC/MS分析", 《应用化学》 * |
| 曾苏: "人尿中美沙酮的分析", 《中国药物依赖性通报》 * |
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| CN106501414A (en) * | 2016-12-07 | 2017-03-15 | 公安部物证鉴定中心 | A kind of method that homogenizes of amphetamine tablet |
| CN106645487A (en) * | 2016-12-28 | 2017-05-10 | 上海微谱化工技术服务有限公司 | Detection and analysis method for methamphetamine in weight-reducing drug |
| CN106645487B (en) * | 2016-12-28 | 2019-12-17 | 上海微谱化工技术服务有限公司 | Detection and analysis method of methamphetamine in weight-reducing drug |
| CN107340347A (en) * | 2017-05-08 | 2017-11-10 | 公安部物证鉴定中心 | Method for preparing purified for the Sauteralgyl standard substance of forensic science illicit drugs inspection |
| CN107340347B (en) * | 2017-05-08 | 2019-11-19 | 公安部物证鉴定中心 | The method for preparing purified of Sauteralgyl standard substance for forensic science illicit drugs inspection |
| CN109507354A (en) * | 2019-01-17 | 2019-03-22 | 浙江工业大学 | The method of Ketamine content in Flash evaporation gas chromatography mass spectrometric determination human hair |
| CN110823855A (en) * | 2019-12-19 | 2020-02-21 | 鄂尔多斯应用技术学院 | Method for rapidly detecting amphetamine drugs in human urine |
| WO2022151842A1 (en) * | 2021-01-14 | 2022-07-21 | 浙江海正药业股份有限公司 | Gas-phase chromatography detection method for dicyclohexylamine in favipiravir |
| CN115060815A (en) * | 2022-05-30 | 2022-09-16 | 广西大学 | Solid phase extraction-liquid chromatography-ion trap/time-of-flight mass spectrometry combined detection method for fluoroamidone metabolites in human urine |
| CN115060815B (en) * | 2022-05-30 | 2023-06-16 | 广西大学 | Solid phase extraction-liquid chromatography-ion trap/time-of-flight mass spectrometry combined detection method for flumidone metabolites in human urine |
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