CN105911177A - GC/MS fast detection method of tetramine in gastric contents in poisoned patients - Google Patents
GC/MS fast detection method of tetramine in gastric contents in poisoned patients Download PDFInfo
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- CN105911177A CN105911177A CN201610234941.0A CN201610234941A CN105911177A CN 105911177 A CN105911177 A CN 105911177A CN 201610234941 A CN201610234941 A CN 201610234941A CN 105911177 A CN105911177 A CN 105911177A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G01N2030/025—Gas chromatography
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Abstract
The invention discloses a GC/MS fast detection method of tetramine in gastric contents in poisoned patients and aims to provide a detection method for detecting tetramine in gastric contents in poisoned patients with high detection sensitivity and short detection period. The method successively comprises the following steps: 1) preparation of a standard solution; 2) preparation of a test sample: fetching 2 ml of gastric contents, adding 4 ml of 10% hydrochloric acid and carrying out eddy mixing for 2 min, centrifuging the mixed solution at the rate of 4000 r/min for 3 min, fetching a supernatant and loading the supernatant through an HLB solid-phase extraction column, discarding, eluting by adding 3 ml of water, discarding an eluant, washing by adding 3 ml of acetonitrile, collecting a flushing fluid, and measuring by an Agilent 7890A-5975C gas chromatograph-mass spectrometer. The invention belongs to the field of a chemical detection technology.
Description
Technical field
The invention discloses the detection method of a kind of Tetramine, specifically, be that a kind of GC/MS quickly detects
The method of the Tetramine in toxic patient gastric content, belongs to technical field of chemical detection.
Background technology
Tetramine (tetramine), chemical entitled tetramethylene-disulfo-tetramine, for quick-acting the killing mouse of severe toxicity
Medicine, colourless, tasteless.It has severe toxicity to all homoiothermic animals, and the Ministry of Agriculture, Ministry of Public Health are once in 1982
Dispatch a joint document in year and forbid to use these compounds as raticide, but still have people to use and cause poisoning.
For providing foundation the most reliably to the diagnoses and treatment of toxic patient, it is necessary to foundation one operation simple and fast,
Qualitative accurate, highly sensitive detection method.Tetramine gas chromatography mass spectrometry method, as uniquely confirming method, does not has
Unified national standard, tradition pretreatment process complexity is loaded down with trivial details, the most long, it usually needs several hours, difficult
To adapt to the quickly poison inspection requirement of public health emergency.And often analyzing complex matrices such as: people
Gastric content time, owing to purifying not, impurity brings system into, makes instrument consume serious, even causes knot
Opinion misjudgment.
Summary of the invention
For the problems referred to above, it is an object of the invention to provide a kind of detection sensitivity high, the detection cycle is short
The detection method of the Tetramine in toxic patient gastric content.
For solving the problems referred to above, the technical scheme that the present invention provides is such that
A kind of GC/MS quickly detects the method for the Tetramine in toxic patient gastric content, includes following successively
Step:
1) preparation of standard solution
Accurately weigh Tetramine standard substance 5.0mg, be placed in 100ml volumetric flask, dissolve and constant volume with acetonitrile,
It is made into 50 μ g/ml contrast solutions；
2) preparation of test sample
Taking gastric content 2ml, add 10% hydrochloric acid 4ml whirlpool mixing 2min, mixed liquor 4000r/min is centrifuged
3MIN, takes supernatant and crosses HLB solid phase extraction column, discard, and add water 3ml eluting, discards eluent,
Adding acetonitrile 3ML to rinse, and collect flushing liquor, upper Agilent 7890A-5975C gas chromatograph-mass spectrometer measures；
Described chromatographic condition is as follows:
Chromatographic column: HP-5MS, 20m × 0.18mm, thickness 0.25 μm；Carrier gas is high-purity helium；Sample introduction
Amount: 50 μ l；During PTV sample introduction, shunting exhaust-valve controls the flow at 80ml/min, and sample introduction completes
After, shunting exhaust-valve closes 1.0min；
Described Mass Spectrometry Conditions is as follows:
Electron impact ion source, electron energy 70eV；Scanning characteristic ion: m/z92, m/z 132, m/z 212,
m/z 240；GC/MS interface temperature: 280 DEG C；Ion source temperature: 230 DEG C；Level Four bar temperature: 150 DEG C.
Further, above-mentioned GC/MS quickly detects the method for the Tetramine in toxic patient gastric content,
Described PTV temperature program(me) is as follows: 40 DEG C maintain 1.0min, rise to 250 DEG C of dimensions with 250 DEG C/min speed
Hold 2min, rise to 300 DEG C with 250 DEG C/min speed and maintain 7min；Column flow rate: with constant current mode 0.5ml/min；
Column oven: 90 DEG C of 2min, rises to 150 DEG C with 100 DEG C/min speed, rises to 280 DEG C with 50 DEG C/min speed
Maintain 4min.
Further, above-mentioned GC/MS quickly detects the method for the Tetramine in toxic patient gastric content,
Described HLB solid phase extraction column uses 3ml methanol, and 3ml water activates.
Further, above-mentioned GC/MS quickly detects the method for the Tetramine in toxic patient gastric content,
Described ammonium acetate pH6.
Compared with prior art, the technical scheme that the present invention provides uses both solid phase extractions to optimize integration,
To reach to improve inspection sensitivity, finding out from the Tetramine standard solution of same concentrations, peak height about exceeds 1.3
Times, it is thus possible to be effectively improved recall rate；Shortening round of visits, retention time about shortens 2 times, thus is
Patient rescues time-consuming；The impact of of low pollution thing, and reduce matrix effect, instrument can be protected.
Accompanying drawing explanation
Fig. 1 is the mass spectrum of SIM type collection Tetramine；
Fig. 2 is the Tetramine standard solution collection of illustrative plates that solid phase extraction combines small-bore chromatograph；
Fig. 3 is the gastric content extracting solution collection of illustrative plates that solid phase extraction combines small-bore chromatograph.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the claim of the present invention is described in further detail, but not
Constitute any limitation of the invention, anyone limited number of time done in the claims in the present invention protection domain
Amendment, still within the claims of the present invention.
The percentage concentration that the present invention relates to, is not particularly illustrated, and liquid is volumetric concentration, solute
Finger mass concentration for solid.
Embodiment 1
1. materials and methods
1.1 instruments and reagent
Agilent 7890A-5975C gas chromatograph-mass spectrometer, is furnished with CTC Multifunctional sample injection device, PTV injection port；
Superpure water machine (ELGAPURELAB ClassicUVF)；Ultrasonic cleaner；High speed centrifuge；C18 is solid
Extract pillar (Tianjin Bonaaijieer Technology Co., Ltd) mutually.
Acetonitrile (HPLC level, Fisher company of the U.S.), other reagent is analytical pure (traditional Chinese medicines group chemistry
Reagent company limited).Experimental water is to filter through ELGAPURELAB ClassicUVF cleaning system
Deionized water；Tetramine standard substance are purchased from State center for standard matter.
1.2 chromatographic condition
Chromatographic column: HP-5MS (20m × 0.18mm thickness 0.25 μm)；Carrier gas is high-purity helium；Sample size:
50μl；During PTV sample introduction (0.8min), shunting exhaust-valve controls the flow at 80ml/min, sample introduction
After completing, shunting exhaust-valve closes (1.0min)；PTV temperature program(me) is as follows: 40 DEG C maintain 1.0min,
Rise to 250 DEG C with 250 DEG C/min speed and maintain 2min, rise to 300 DEG C with 250 DEG C/min speed and maintain 7min.
Column flow rate: with constant current mode 0.5ml/min.Column oven: 90 DEG C (2min), with 100 DEG C/min speed liter
To 150 DEG C, rise to 280 DEG C with 50 DEG C/min speed and maintain 4min.
Use solvent purging function and the HP-5MS (20m × 0.18mm thickness 0.25 μm) of PTV injection port,
Appearance time can be accelerated, thus reduces analysis time on the basis of ensureing sensitivity.
Shunting Splitless injecting samples mouth relative to common injector with common gas phase, general effective sample size is 1
μl；But the application have employed large volume sample injection (50ul) and PTV sample introduction pattern, for reaching to be not required to after extracting
Extracting solution is concentrated, gets final product loading, and realize solvent purging at injection port end, after making object focus on
Enter chromatographic column, be greatly saved the time of pre-treatment.
2.3 Mass Spectrometry Conditions
Electron bombardment (EI) ion source, electron energy 70eV；Scanning characteristic ion: m/z92, m/z 132,
M/z 212, m/z 240 (mass spectrum is shown in Fig. 1)；GC/MS interface temperature: 280 DEG C；Ion source temperature:
230℃；Level Four bar temperature: 150 DEG C.
The preparation of 2.4 standard solution
Accurately weigh Tetramine standard substance 5.0mg, be placed in 100ml volumetric flask, dissolve and constant volume with acetonitrile,
It is made into 50 μ g/ml contrast solutions.
The preparation of 2.5 test samples
Take gastric content 2ml, add 10% hydrochloric acid (PH6) 4ml whirlpool mixing 2min, mixed liquor 4000r/min
Centrifugal 3MIN, takes supernatant (about 4ml) and crosses HLB solid phase extraction column (3ml methanol, 3ml water activates),
Discarding, add water 3ml eluting, discards eluent, adds acetonitrile 3ML and rinses, and collects flushing liquor, upper gas
Matter combined instrument measures.
3 results
Being added in blank gastric content sample by Tetramine, " 2.5 " the joint method of employing processes, and measures poison
Mus by force in the gastric content response rate, every kind of addition level determination 3 times, average and detect as reality,
The results are shown in Table 1.
The response rate is 85%～96%, and method accuracy rate is high.
Claims (4)
1. a method for the Tetramine during GC/MS quickly detects toxic patient gastric content, its feature exists
In, comprise the steps: successively
1) preparation of standard solution
Accurately weigh Tetramine standard substance 5.0mg, be placed in 100ml volumetric flask, dissolve and constant volume with acetonitrile,
It is made into 50 μ g/ml contrast solutions；
2) preparation of test sample
Taking gastric content 2ml, add 10% hydrochloric acid 4ml whirlpool mixing 2min, mixed liquor 4000r/min is centrifuged
3MIN, takes supernatant and crosses HLB solid phase extraction column, discard, and add water 3ml eluting, discards eluent,
Adding acetonitrile 3ML to rinse, and collect flushing liquor, upper Agilent 7890A-5975C gas chromatograph-mass spectrometer measures；
Described chromatographic condition is as follows:
Chromatographic column: HP-5MS, 20m × 0.18mm, thickness 0.25 μm；Carrier gas is high-purity helium；Sample introduction
Amount: 50 μ l；During PTV sample introduction, shunting exhaust-valve controls the flow at 80ml/min, and sample introduction completes
After, shunting exhaust-valve closes 1.0min；
Described Mass Spectrometry Conditions is as follows:
Electron impact ion source, electron energy 70eV；Scanning characteristic ion: m/z92, m/z 132, m/z 212,
m/z 240；GC/MS interface temperature: 280 DEG C；Ion source temperature: 230 DEG C；Level Four bar temperature: 150 DEG C.
GC/MS the most according to claim 1 quickly detects the Tetramine in toxic patient gastric content
Method, it is characterised in that described PTV temperature program(me) is as follows: 40 DEG C maintain 1.0min, with 250 DEG C
/ min speed rises to 250 DEG C and maintains 2min, rises to 300 DEG C with 250 DEG C/min speed and maintains 7min；Post stream
Speed: with constant current mode 0.5ml/min；Column oven: 90 DEG C of 2min, rises to 150 DEG C with 100 DEG C/min speed,
Rise to 280 DEG C with 50 DEG C/min speed and maintain 4min.
GC/MS the most according to claim 1 quickly detects the Tetramine in toxic patient gastric content
Method, it is characterised in that described HLB solid phase extraction column uses 3ml methanol, and 3ml water activates.
GC/MS the most according to claim 1 quickly detects the Tetramine in toxic patient gastric content
Method, it is characterised in that described ammonium acetate pH6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114716556A (en) * | 2020-12-22 | 2022-07-08 | 中国农业大学 | Rat-poisoning nano antibody and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507794A (en) * | 2011-11-24 | 2012-06-20 | 重庆警官职业学院 | Method for rapidly detecting poisoned substances by adopting urine |
| CN104965038A (en) * | 2015-04-27 | 2015-10-07 | 公安部物证鉴定中心 | Method for screening toxic substances in sample by using solid phase microextraction-GC-MS |
-
2016
- 2016-04-15 CN CN201610234941.0A patent/CN105911177A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507794A (en) * | 2011-11-24 | 2012-06-20 | 重庆警官职业学院 | Method for rapidly detecting poisoned substances by adopting urine |
| CN104965038A (en) * | 2015-04-27 | 2015-10-07 | 公安部物证鉴定中心 | Method for screening toxic substances in sample by using solid phase microextraction-GC-MS |
Non-Patent Citations (4)
| Title |
|---|
| ELIZABETH HAMELIN 等: "Quantitation of tetramethylene disulfotetramine in human urine using isotope dilution gas chromatography mass spectrometry (GC/MS and GC/MS/MS)", 《JOURNAL OF CHROMATOGRAPHY B》 * |
| 林佶 等: "GC/MS定性定量分析人血尿食物中的毒鼠强", 《实用预防医学》 * |
| 牛文凯 等: "急性中毒患者血液毒鼠强的GC/MS检测及临床应用", 《中国医刊》 * |
| 罗达龙 等: "气质联用法快速检测中毒患者体液中毒鼠强", 《食品安全质量检测学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114716556A (en) * | 2020-12-22 | 2022-07-08 | 中国农业大学 | Rat-poisoning nano antibody and application thereof |
| CN114716556B (en) * | 2020-12-22 | 2023-03-24 | 中国农业大学 | Rat-poisoning nano antibody and application thereof |
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