CN102226794A - Liquid chromatography-tandom mass spectrometry detection method of thirty-one drugs in human blood - Google Patents
Liquid chromatography-tandom mass spectrometry detection method of thirty-one drugs in human blood Download PDFInfo
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Abstract
The invention relates to a liquid chromatography-tandom mass spectrometry detection method of common drugs in human blood. According to the method of the invention, an extraction method, a purification method, chromatographic conditions and mass spectral conditions of the thirty-one common drugs in the human blood are established. The method has a minimum detection limit of 1 to 2 ng/ml. When the concentration is from 2 to 100 ng/ml, the linearity is good with a related coefficient of 0.9771 to 0.9995 and an RSD of less than 13.2%. The method of the present invention has the advantages of strong pertinence, simple operation, fast detection speed, wide detection area, and easy popularization and application, can be used for fast detection of entry-exit inspection and quarantine departments, disease control centers and police departments, and positive result confirmation. The drugs can be detected through blood sampling, so a detection escape phenomenon which may appear when entry-exit inspection and quarantine systems guard passes at ports is prevented.
Description
Technical field
The present invention relates to a kind of detection method of drugs, the liquid chromatography-tandem mass spectrometry detection method of 31 kinds of drugs in particularly a kind of human blood.
Background technology
Drug abuse, traffic in drugs have become global social effects of pollution.In a single day the people is infected with drugs. among the deformity " pleasant sensation " that will often wallow in drugs and had fantasies of out, be not in the mood for working and learning.Take drugs and also can cause a series of family social problem.In view of consume illegal drugs to family, particularly to the serious harm of society, abroad some countries are except that taking the corresponding control measures national drug addict, the proof that provides the applicant not take drugs also are provided the immigrant, as Russia.Along with global economic integration progress is accelerated, other countries inevitably will put into effect similar regulation successively to the immigrant.Relating to the health status aspect when responding actively more external countries to my personnel's entry visa proposes to add and does the requirement that drugs detect, inspection and quarantine department will actively carry out material and technical preparation to tackle external requirement to my entry personnel's health examination on the one hand according to the requirement of State Bureau; From the protection China's people's health and the purpose of maintaining social stability, also should take the principle of equity on the other hand, the personnel of coming to China are increased the requirement that drugs detect.
The measuring technology of the interior drug ingredient check of the most widely used human body both at home and abroad is immunoassay technology and vapor-phase chromatography (GC) at present, and (GC/MS) that uses gas chromatography mass spectrometry to detect abroad also arranged.Retrieval Chinese Industrial Standards (CIS) net finds that the industry standard about a few class drugs such as morphine, cocaine, heroin of the Ministry of Public Security is only arranged in standard, mainly be direct detection to drugs, and is not the detection method at the body fluid aspect.The method that present inspection and quarantine department carries out the drugs detection to inward and outward personnel's urine mainly adopts colloidal gold technique fast detecting morphine and meth, and false positive rate is high, and can only detect 2 kinds of drugs.Therefore set up a kind of fast, sensitive, accurately multiple drugs simultaneously detection method become particularly important.
Summary of the invention
Technical matters to be solved by this invention is at the deficiencies in the prior art, provide that a kind of method is with strong points, simple to operate, detection speed is fast, it is wide to detect, reduced testing cost, the liquid chromatography-tandem mass spectrometry detection method of 31 kinds of drugs in the human blood that is easy to apply.
Technical matters to be solved by this invention is to realize by following technical scheme.The present invention is the liquid chromatography-tandem mass spectrometry detection method of 31 kinds of drugs in a kind of human blood, is characterized in, its step is as follows:
(1) sample preparation: take by weighing the 2g sample, be accurate to 0.01g, place 50mL tool plug centrifuge tube, add 1mL 0.1mol/L NaOH solution earlier, add 10mL ethyl acetate again, abundant mixing 1min on the liquid vortex mixer, with the centrifugal 10min of 4000r/min, draw upper strata ethyl acetate in test tube; Add 0.2mL 1.0mol/LNaH
2PO
4After, behind abundant mixing on the liquid vortex mixer, add 10mL ethyl acetate and repeat to extract once, merge extracted twice liquid; Extract dries up instrument with nitrogen and dries up at 40 ℃; Adding 1mL volume ratio is 30: 70 a methyl alcohol: eddies of water supination behind the 0.25 μ m filter membrane, gets testing sample excessively;
(2) measure: testing sample is measured with liquid chromatography-series connection quadrupole mass spectrometer; In the liquid chromatography-tandem mass spectrometry analytic approach of 31 kinds of drugs, except barbiturate used the negative ion mode analysis, all the other compounds all used the positive ion mode analysis; The mass spectrum condition of positive ion mode is:
Ionization source: ESI source; Scan pattern: positive ion is selected scan pattern SRM;
Electron spray voltage: 2.5kV; Dry gas temperature: 400 ℃; Gas curtain atmospheric pressure: 45arb;
Assist gas pressure power: 7arb; Capillary temperature: 350 ℃; Collision gas: high-purity argon gas;
The mass spectrum condition of negative ion mode is:
Ionization source: ESI source; Scan pattern: negative ion is selected scan pattern SRM;
Electron spray voltage: 2.5kV; Dry gas temperature: 400 ℃; Gas curtain atmospheric pressure: 50arb;
Assist gas pressure power: 7arb; Capillary temperature: 320 ℃; Collision gas: high-purity argon gas;
Chromatographic condition is:
Chromatographic column: Phenomenex Gemini C18100 * 2.0,3 μ m;
Column temperature: room temperature; Flow velocity: 250 μ L/min; Sampling volume: 25 μ L;
The eluent gradient of negative ions pattern sees Table 1 and table 2;
Table 1. positive ion mode eluent gradient
Table 2. negative ion mode eluent gradient
The title of 31 kinds of drugs, monitoring ion pair and collision energy see Table 3, and band *'s is quota ion;
The Sino-British literary fame of 31 kinds of drugs of table 3 and selection ion
Qualitative-and-quantitative method is: the abundance ratio with the monitoring ion pair of the relative retention time of each drugs and each drugs is qualitative foundation, and the retention time of each drugs sees Table 3; Quantitative with external standard method, calculate its residual quantity in sample with the peak area or the peak height of each drugs.
The computing formula of residual quantity is as follows:
In the formula:
Drugs content in the R-sample (μ g/g)
C
Mark-standard model concentration (μ g/mL)
V
Mark-standard model sample size (μ L)
V
EventuallyThe final constant volume of-sample solution (mL)
V
Sample-sample solution sampling volume (μ L)
S
Sample(H
Sample)-the inject peak area (mm of standard solution
2) or (peak height) is (mm)
S
Mark(H
MarkPeak area (the mm of)-injecting sample solution
2) or (peak height) is (mm)
L
1The total amount of-extract (mL)
L
2The amount of taking of-extract (mL)
W-sample weighting amount (g).
Compared with prior art, the inventive method has the following advantages:
1, detection method of the present invention adopts the method for liquid-liquid extraction to extract and purify, and realizes albuminous degeneration and regulate the pH value that by adding sodium hydroxide solution the ethyl acetate liquid-liquid extraction is extracted.Simple to operation, good purification, the recycled in its entirety rate is good, has saved organic solvent and processing time simultaneously, has simplified the pre-treatment process of sample.
2, detection method of the present invention adopts the online valve of C18 post to switch and purifies the tandem mass spectrum analysis.Because the kind of the drugs that relate to is more, be difficult to when further purifying again select a kind of solid-phase extraction column to reach satisfied result.Online switching by chromatographic column purifies, and is used for reducing the pollution of sample to mass spectrometer.Concrete way is exactly by the online transfer valve on the mass spectrometer, before all compounds of analyzing do not go out the peak and after all components all flowed out chromatographic column, the solution that chromatographic column is flowed out switches in the waste liquid, do not advance mass spectrophotometry, a mass spectrum analysis bank distributes the effluent of this time period.The compound of the salt of a large amount of low reservation before component flows out like this and impurity and the strong low pole that keeps does not all enter mass spectral ion gun, has effectively reduced sample to mass spectral pollution.
3, the inventive method is selected alkali-proof chromatographic column for use, and ammoniacal liquor is regulated moving phase pH value, and the chromatogram that improves morphine keeps.
4, the method minimum detectability reaches 1-2 μ g/kg.In the 2-100ng/mL concentration range, more than 30 kind of drugs are linear good, and related coefficient is 0.9771-0.9995.Between 70%-110%, RSD is less than 13.2% in the recovery of part drugs.
5, detection method of the present invention has been set up the detection method of 31 kinds of common drugs in the liquid chromatography-tandem mass spectrometry method detection human blood.31 kinds of drugs of disposable analysis, method is with strong points, simple to operate, detection speed fast, it is wide to detect, reduced testing cost, is easy to apply.The conclusive evidence that can be used for inspection and quarantining for import/export, Center for Disease Control, public security department's fast detecting and positive findings.The detection drugs of can taking a blood sample, contingently when preventing that entry and exit inspections inspection and quarantine system port from checking on escape to examine phenomenon and take place, the strong ability of checking on that improves the inspection and quarantine system provides reference for being engaged in testing of inward and outward personnel's drugs and formulation relevant industries and national standard.
Embodiment
Below further describe concrete technical scheme of the present invention,, and do not constitute restriction its right so that those skilled in the art understands the present invention further.
Embodiment 1.The liquid chromatography-tandem mass spectrometry detection method of 31 kinds of drugs in the human blood, its step is as follows:
(1) sample preparation: take by weighing the 2g sample, be accurate to 0.01g, place 50mL tool plug centrifuge tube, add 1mL 0.1mol/L NaOH solution earlier, add 10mL ethyl acetate again, abundant mixing 1min on the liquid vortex mixer, with the centrifugal 10min of 4000r/min, draw upper strata ethyl acetate in test tube; Add 0.2mL 1.0mol/LNaH
2PO
4After, behind abundant mixing on the liquid vortex mixer, add 10mL ethyl acetate and repeat to extract once, merge extracted twice liquid; Extract dries up instrument with nitrogen and dries up at 40 ℃; Adding 1mL volume ratio is 30: 70 a methyl alcohol: eddies of water supination behind the 0.25 μ m filter membrane, gets testing sample excessively;
(2) measure: testing sample is measured with liquid chromatography-series connection quadrupole mass spectrometer; In the liquid chromatography-tandem mass spectrometry analytic approach of 31 kinds of drugs, except barbiturate used the negative ion mode analysis, all the other compounds all used the positive ion mode analysis; The mass spectrum condition of positive ion mode is:
Ionization source: ESI source; Scan pattern: positive ion is selected scan pattern SRM;
Electron spray voltage: 2.5kV; Dry gas temperature: 400 ℃; Gas curtain atmospheric pressure: 45arb;
Assist gas pressure power: 7arb; Capillary temperature: 350 ℃; Collision gas: high-purity argon gas;
The mass spectrum condition of negative ion mode is:
Ionization source: ESI source; Scan pattern: negative ion is selected scan pattern SRM;
Electron spray voltage: 2.5kV; Dry gas temperature: 400 ℃; Gas curtain atmospheric pressure: 50arb;
Assist gas pressure power: 7arb; Capillary temperature: 320 ℃; Collision gas: high-purity argon gas;
Chromatographic condition is:
Chromatographic column: Phenomenex Gemini C18100 * 2.0,3 μ m;
Column temperature: room temperature; Flow velocity: 250 μ L/min; Sampling volume: 25 μ L;
The eluent gradient of negative ions pattern sees Table 1 and table 2;
Table 1. positive ion mode eluent gradient
Table 2. negative ion mode eluent gradient
The title of 31 kinds of drugs, monitoring ion pair and collision energy see Table 3, and band *'s is quota ion;
The Sino-British literary fame of 31 kinds of drugs and selection ion
Qualitative-and-quantitative method is: the abundance ratio with the monitoring ion pair of the relative retention time of each drugs and each drugs is qualitative foundation, and the retention time of each drugs sees Table 3; Quantitative with external standard method, calculate its residual quantity in sample with the peak area or the peak height of each drugs.
The test experience that adopts the present embodiment method to carry out.
Lianyun Harbour inspection and quarantine bureau went to Russian personnel to carry out the drugs detection in 2010 to 144, detected crystal methamphetamine and morphine by the Russian side requirement, and method is colloidal gold immunity chromatography and present embodiment method.Find doubtful morphine 1 example with colloidal gold immunity chromatography, prove conclusively that confirmed results shows that the blood concentration of morphine is 28 μ g/kg with the present embodiment method.Through investigating the pectoral (compound codeine phosphate) of having taken certain company before this labour service for export personnel stop inspection,, and produce morphine after the codeine metabolism because this oral liquid contains codeine.Cut out this medicine after 2 days, negative with these two method testing results.Proof present embodiment method accurately and reliably.
Claims (1)
1. the liquid chromatography-tandem mass spectrometry detection method of 31 kinds of drugs in the human blood is characterized in that its step is as follows:
(1) sample preparation: take by weighing the 2g sample, be accurate to 0.01g, place 50mL tool plug centrifuge tube, add 1mL 0.1mol/L NaOH solution earlier, add 10mL ethyl acetate again, abundant mixing 1min on the liquid vortex mixer, with the centrifugal 10min of 4000r/min, draw upper strata ethyl acetate in test tube; Add 0.2mL 1.0mol/LNaH
2PO
4After, behind abundant mixing on the liquid vortex mixer, add 10mL ethyl acetate and repeat to extract once, merge extracted twice liquid; Extract dries up instrument with nitrogen and dries up at 40 ℃; Adding 1mL volume ratio is 30: 70 a methyl alcohol: eddies of water supination behind the 0.25 μ m filter membrane, gets testing sample excessively;
(2) measure: testing sample is measured with liquid chromatography-series connection quadrupole mass spectrometer; In the liquid chromatography-tandem mass spectrometry analytic approach of 31 kinds of drugs, except barbiturate used the negative ion mode analysis, all the other compounds all used the positive ion mode analysis; The mass spectrum condition of positive ion mode is:
Ionization source: ESI source; Scan pattern: positive ion is selected scan pattern SRM;
Electron spray voltage: 2.5kV; Dry gas temperature: 400 ℃; Gas curtain atmospheric pressure: 45arb;
Assist gas pressure power: 7arb; Capillary temperature: 350 ℃; Collision gas: high-purity argon gas;
The mass spectrum condition of negative ion mode is:
Ionization source: ESI source; Scan pattern: negative ion is selected scan pattern SRM;
Electron spray voltage: 2.5kV; Dry gas temperature: 400 ℃; Gas curtain atmospheric pressure: 50arb;
Assist gas pressure power: 7arb; Capillary temperature: 320 ℃; Collision gas: high-purity argon gas;
Chromatographic condition is:
Chromatographic column: Phenomenex Gemini C18100 * 2.0,3 μ m;
Column temperature: room temperature; Flow velocity: 250 μ L/min; Sampling volume: 25 μ L;
The eluent gradient of negative ions pattern sees Table 1 and table 2;
Table 1. positive ion mode eluent gradient
Table 2. negative ion mode eluent gradient
The title of 31 kinds of drugs, monitoring ion pair and collision energy see Table 3, and band *'s is quota ion;
The Sino-British literary fame of 31 kinds of drugs and selection ion
Qualitative-and-quantitative method is: the abundance ratio with the monitoring ion pair of the relative retention time of each drugs and each drugs is qualitative foundation, and the retention time of each drugs sees Table 3; Quantitative with external standard method, calculate its residual quantity in sample with the peak area or the peak height of each drugs.
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| CN106053426A (en) * | 2016-05-13 | 2016-10-26 | 中国科学院合肥物质科学研究院 | Method for detecting drugs in human body fluids based on surface enhanced Raman spectrum technology |
| CN106404925A (en) * | 2015-07-31 | 2017-02-15 | 复旦大学 | Method for determining six barbiturates in human whole blood |
| CN107202840A (en) * | 2017-05-23 | 2017-09-26 | 上海应用技术大学 | A kind of method for detecting 4 kinds of barbiturates downerns of fresh milk |
| CN107478747A (en) * | 2017-05-10 | 2017-12-15 | 山东省公安厅 | The liquid chromatography mass screening method of unknown poisonous substance in blood |
| CN107741464A (en) * | 2017-11-27 | 2018-02-27 | 浙江公正检验中心有限公司 | 22 kinds of illegal detection methods for adding class drug residue of calming the nerves in health products |
| CN107764916A (en) * | 2017-09-28 | 2018-03-06 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | The method of analgin, 4 (methylamino) antipyrines and caffeine in one kind detection herbal tea |
| CN107807178A (en) * | 2016-09-08 | 2018-03-16 | 中国民用航空局民用航空医学中心 | Septicemia product and resisting mental disease class medicine liquid chromatography-mass spectrography detection method |
| CN109613126A (en) * | 2018-11-01 | 2019-04-12 | 中国环境科学研究院 | The measuring method of illicit drug and its metabolite in a kind of fish body |
| CN109828039A (en) * | 2018-12-20 | 2019-05-31 | 广州市圣鑫生物科技有限公司 | The kit of common illicit drugs inspection, pre-treating method and detection method in hair |
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Cited By (15)
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| CN106404925A (en) * | 2015-07-31 | 2017-02-15 | 复旦大学 | Method for determining six barbiturates in human whole blood |
| CN106404925B (en) * | 2015-07-31 | 2019-06-21 | 复旦大学 | The method for measuring 6 kinds of barbiturates in people's whole blood |
| CN106053426A (en) * | 2016-05-13 | 2016-10-26 | 中国科学院合肥物质科学研究院 | Method for detecting drugs in human body fluids based on surface enhanced Raman spectrum technology |
| CN106053426B (en) * | 2016-05-13 | 2019-07-19 | 中国科学院合肥物质科学研究院 | Method based on drugs in Surface enhanced Raman spectroscopy technology detection human body fluid |
| CN107807178A (en) * | 2016-09-08 | 2018-03-16 | 中国民用航空局民用航空医学中心 | Septicemia product and resisting mental disease class medicine liquid chromatography-mass spectrography detection method |
| CN107807178B (en) * | 2016-09-08 | 2020-09-18 | 中国民用航空局民用航空医学中心 | Liquid chromatography-mass spectrometry detection method for drugs and anti-psychotic drugs in blood |
| CN107478747A (en) * | 2017-05-10 | 2017-12-15 | 山东省公安厅 | The liquid chromatography mass screening method of unknown poisonous substance in blood |
| CN107478747B (en) * | 2017-05-10 | 2019-11-08 | 山东省公安厅 | The liquid chromatography-mass spectrography screening method of unknown poisonous substance in blood |
| CN107202840B (en) * | 2017-05-23 | 2019-06-28 | 上海应用技术大学 | A method of detection 4 kinds of barbiturates downerns of fresh milk |
| CN107202840A (en) * | 2017-05-23 | 2017-09-26 | 上海应用技术大学 | A kind of method for detecting 4 kinds of barbiturates downerns of fresh milk |
| CN107764916A (en) * | 2017-09-28 | 2018-03-06 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | The method of analgin, 4 (methylamino) antipyrines and caffeine in one kind detection herbal tea |
| CN107741464A (en) * | 2017-11-27 | 2018-02-27 | 浙江公正检验中心有限公司 | 22 kinds of illegal detection methods for adding class drug residue of calming the nerves in health products |
| CN109613126A (en) * | 2018-11-01 | 2019-04-12 | 中国环境科学研究院 | The measuring method of illicit drug and its metabolite in a kind of fish body |
| CN109613126B (en) * | 2018-11-01 | 2020-11-03 | 中国环境科学研究院 | Method for determining illegal drugs and metabolites thereof in fish body |
| CN109828039A (en) * | 2018-12-20 | 2019-05-31 | 广州市圣鑫生物科技有限公司 | The kit of common illicit drugs inspection, pre-treating method and detection method in hair |
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