CN105651926A - Method for detecting tetramine in urine of poisoning patients by gas chromatography-mass spectrometry - Google Patents

Method for detecting tetramine in urine of poisoning patients by gas chromatography-mass spectrometry Download PDF

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Publication number
CN105651926A
CN105651926A CN201610235130.2A CN201610235130A CN105651926A CN 105651926 A CN105651926 A CN 105651926A CN 201610235130 A CN201610235130 A CN 201610235130A CN 105651926 A CN105651926 A CN 105651926A
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Prior art keywords
tetramine
urine
mass spectrometry
gas chromatography
rises
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CN201610235130.2A
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Inventor
陈学松
罗达龙
刘慧妍
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Wuzhou Institutes for Food and Drug Control
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Wuzhou Institutes for Food and Drug Control
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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
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • 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
    • 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
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • 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
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025—Gas chromatography
    • 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
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N2030/062—Preparation extracting sample from raw material
    • 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
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
    • G01N2030/8813—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample biological materials

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Investigating Or Analysing Biological Materials (AREA)

Abstract

The invention discloses a method for detecting tetramine in urine of poisoning patients by gas chromatography-mass spectrometry and aims at providing a method for determining the tetramine in the urine of the poisoning patients, which is simple, easy and rapid to operate and is accurately qualitative. The method comprises the following steps in sequence: (1) preparing a standard liquid accurately weighing 5.0mg of a tetramine standard product and putting the tetramine standard product into a 100-ml volumetric flask; dissolving with acetone and making the volume constant to prepare a 50mu g/ml contrast sliquid; and (2) preparing a test sample: taking 5ml of the urine and putting the urine into a 15ml centrifugal tube; adding 5ml of the acetone and carrying out vortex shaking for 2 minutes; and centrifuging for 5 minutes at the speed of 4000r/min, and taking liquid supernatant and determining on a liquid chromatograph-mass spectrometer. The method disclosed by the invention belongs to the technical field of chemical detection.

Description

The method of the Tetramine in gas chromatography mass spectrometry detection toxic patient urine
Technical field
The invention discloses the detection method of a kind of Tetramine, specifically, be the method for Tetramine in a kind of gas chromatography mass spectrometry detection toxic patient urine, belong to technical field of chemical detection.
Background technology
Tetramine (tetramine), chemistry tetramethylene-disulfo-tetramine by name, for the raticide that severe toxicity is quick-acting, colourless, tasteless. All homoiothermic animals are had severe toxicity by it, and the Ministry of Agriculture, Ministry of Public Health were once dispatched a joint document in nineteen eighty-two and forbidden to use these compounds as raticide, but still had people to use and cause poisoning. For providing in time reliably foundation to the diagnoses and treatment of toxic patient, it is necessary to set up and a kind of operate simple and fast, qualitative accurate, highly sensitive detection method. Tetramine gas chromatography mass spectrometry method is as uniquely confirming method, it does not have unified national standard, and tradition pretreatment process complexity is loaded down with trivial details, consuming time long, it usually needs several hours, it is difficult to adapt to the quickly poison inspection requirement of public health emergency. And often when analyzing complex matrices urine, owing to purifying not, impurity brings system into, make instrument consume serious, even cause conclusion misjudgment.
Summary of the invention
For the problems referred to above, it is an object of the invention to provide a kind of method operating simple and fast, the qualitative Tetramine measured accurately in toxic patient urine.
For solving the problems referred to above, technical scheme provided by the invention is such that
The method of the Tetramine in a kind of gas chromatography mass spectrometry detection toxic patient urine, comprises the steps: successively
1) preparation of standard solution
Accurately weigh Tetramine standard substance 5.0mg, be placed in 100ml volumetric flask, with acetone solution constant volume, be made into 50 �� g/ml contrast solutions.
2) preparation of test sample
Take urine 5ml and put in 15ml centrifuge tube, add 5ml acetone, whirlpool concussion 2min; 4000r/min is centrifuged 5min, takes gas chromatograph-mass spectrometer on supernatant and measures.
Further, the method for the above-mentioned Tetramine in gas chromatography mass spectrometry detection toxic patient urine, described gas chromatograph-mass spectrometer adopts Agilent 7890A-5975C gas chromatograph-mass spectrometer.
Further, the method for the above-mentioned Tetramine in gas chromatography mass spectrometry detection toxic patient urine, described chromatographic condition is as follows:
Chromatographic column: HP-5MS, 20m �� 0.18mm, thickness 0.18 ��m;Carrier gas is high-purity helium; Sample size: 50 �� l; During PTV sample introduction, shunting exhaust-valve controls the flow at 80ml/min, and after sample introduction completes, 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/z132, m/z212, m/z240 (; GC/MS interface temperature: 280 DEG C; Ion source temperature: 230 DEG C; Level Four bar temperature: 150 DEG C.
Further, the method of the above-mentioned Tetramine in gas chromatography mass spectrometry detection toxic patient urine, described PTV temperature program(me) is as follows: 40 DEG C maintain 1.0min, rises to 250 DEG C with 250 DEG C/min speed and maintains 2min, rises to 300 DEG C with 250 DEG C/min speed and maintains 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 and maintains 4min.
Compared with prior art, the application establishes utilization liquid-liquid extraction and carries out the urine of tetramine poisoning patient purifying pre-treatment, in conjunction with large volume sample injection, PTV sample introduction, carries out Tetramine detection confirmation by sim pattern. Overall process about 20min consuming time is completed from sample pre-treatments to confirmation. The method tool operation simple and fast, qualitative accurate, sensitivity high, can apply to emergent inspection, save valuable time for patient's rescue work, decrease the use of high-purity helium, both reduced cost, decreased discharging of waste liquid, there is important environment protection significance.
Accompanying drawing explanation
Fig. 1 is the mass spectrum of SIM type collection Tetramine;
Fig. 2 is the liquid-liquid extraction method Tetramine standard solution collection of illustrative plates in conjunction with heavy caliber chromatographic column;
Fig. 3 is the liquid-liquid extraction method urine extracting solution collection of illustrative plates in conjunction with heavy caliber chromatographic column;
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 constituting any limitation of the invention, the amendment of anyone limited number of time made in the claims in the present invention protection domain, still within the claims of the present invention.
The percentage concentration that the present invention relates to, it does not have special instruction, liquid is volumetric concentration, and solute is the finger mass concentration of 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 (ELGAPURELABClassicUVF); Ultrasonic cleaner; High speed centrifuge; C18 solid phase extraction column (Tianjin Bonaaijieer Technology Co., Ltd)
Acetone (HPLC level, Fisher company of the U.S.), other reagent is analytical pure (Chemical Reagent Co., Ltd., Sinopharm Group); Experimental water is the deionized water filtered through ELGAPURELABClassicUVF cleaning system; Tetramine standard substance are purchased from State center for standard matter.
1.2 chromatographic conditions
Chromatographic column: HP-5MS (20m �� 0.18mm thickness 0.18 ��m); Carrier gas is high-purity helium; Sample size: 50 �� l; During PTV sample introduction (0.8min), shunting exhaust-valve controls the flow at 80ml/min, and after sample introduction completes, shunting exhaust-valve closes (1.0min); PTV temperature program(me) is as follows: 40 DEG C maintain 1.0min, rises to 250 DEG C with 250 DEG C/min speed and maintains 2min, rises to 300 DEG C with 250 DEG C/min speed and maintains 7min. Column flow rate: with constant current mode 0.5ml/min. Column oven: 90 DEG C (2min), rises to 150 DEG C with 100 DEG C/min speed, rises to 280 DEG C with 50 DEG C/min speed and maintains 4min
The solvent adopting PTV injection port purges function and HP-5MS (20m �� 0.18mm thickness 0.18 ��m), ensureing on the basis of sensitivity, can accelerate appearance time, thus reducing analysis time.
Relative to common injector and common gas phase shunting Splitless injecting samples mouth, general effective sample size is 1 �� l; But the application have employed large volume sample injection (50ul) and PTV sample introduction pattern, for not needing extracting solution is concentrated after reaching extraction, get final product loading, and realize solvent purging at injection port end, make object enter chromatographic column after focusing on, be greatly saved the time of pre-treatment.
1.3 Mass Spectrometry Conditions
Electron bombardment (EI) ion source, electron energy 70eV; Scanning characteristic ion: m/z92, m/z132, m/z212, m/z240 (mass spectrum is shown in Fig. 1); GC/MS interface temperature: 280 DEG C; Ion source temperature: 230 DEG C; Level Four bar temperature: 150 DEG C.
The preparation of 1.4 standard solution
Accurately weigh Tetramine standard substance 5.0mg, be placed in 100ml volumetric flask, with acetone solution constant volume, be made into 50 �� g/ml contrast solutions.
The preparation of 1.5 test samples
Take urine 5ml and put in 15ml centrifuge tube, add 5ml acetone, whirlpool concussion 2min; 4000r/min is centrifuged 5min, takes gas chromatograph-mass spectrometer on supernatant and surveys.
2 results
Being added by Tetramine in blank diaper sample, " 1.5 " the joint method of employing processes, and measures the Tetramine response rate in urine, every kind of addition level determination 3 times, averages and detects as reality, and result is in Table 1.
Result shows that the urine response rate is 85%��96%, and method accuracy rate is high.

Claims (4)

1. the method for the Tetramine in a gas chromatography mass spectrometry detection toxic patient urine, it is characterised in that comprise the steps: successively
1) preparation of standard solution
Accurately weigh Tetramine standard substance 5.0mg, be placed in 100ml volumetric flask, with acetone solution constant volume, be made into 50 �� g/ml contrast solutions;
2) preparation of test sample
Take urine 5ml and put in 15ml centrifuge tube, add 5ml acetone, whirlpool concussion 2min; 4000r/min is centrifuged 5min.
2. the method for the Tetramine in gas chromatography mass spectrometry according to claim 1 detection toxic patient urine, it is characterised in that described gas chromatograph-mass spectrometer adopts Agilent 7890A-5975C gas chromatograph-mass spectrometer.
3. the method for the Tetramine in gas chromatography mass spectrometry according to claim 1 detection toxic patient urine, it is characterised in that described chromatographic condition is as follows:
Chromatographic column: HP-5MS, 20m �� 0.18mm, thickness 0.18 ��m; Carrier gas is high-purity helium; Sample size: 50 �� l; During PTV sample introduction, shunting exhaust-valve controls the flow at 80ml/min, and after sample introduction completes, 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/z132, m/z212, m/z240 (; GC/MS interface temperature: 280 DEG C; Ion source temperature: 230 DEG C; Level Four bar temperature: 150 DEG C.
4. the method for the Tetramine in gas chromatography mass spectrometry according to claim 1 detection toxic patient urine, it is characterized in that, described PTV temperature program(me) is as follows: 40 DEG C maintain 1.0min, rises to 250 DEG C with 250 DEG C/min speed and maintains 2min, rises to 300 DEG C with 250 DEG C/min speed and maintains 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 and maintains 4min.
CN201610235130.2A 2016-04-15 2016-04-15 Method for detecting tetramine in urine of poisoning patients by gas chromatography-mass spectrometry Pending CN105651926A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0321863A (en) * 1989-06-19 1991-01-30 Shimadzu Corp Method and apparatus for analyzing triethylene tetramine or the like
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
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0321863A (en) * 1989-06-19 1991-01-30 Shimadzu Corp Method and apparatus for analyzing triethylene tetramine or the like
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
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 (2)

* Cited by examiner, † Cited by third party
Title
廖华勇 等: "大体积进样气质联用法同时检测毒鼠强和氟乙酰胺", 《色谱》 *
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》 *

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Application publication date: 20160608