CN102297891A - Method for rapidly detecting diphacinone or diphacinone sodium salt in beverage - Google Patents
Method for rapidly detecting diphacinone or diphacinone sodium salt in beverage Download PDFInfo
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- CN102297891A CN102297891A CN2010102069094A CN201010206909A CN102297891A CN 102297891 A CN102297891 A CN 102297891A CN 2010102069094 A CN2010102069094 A CN 2010102069094A CN 201010206909 A CN201010206909 A CN 201010206909A CN 102297891 A CN102297891 A CN 102297891A
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Abstract
The invention discloses a method for rapidly and sensitively detecting diphacinone or diphacinone sodium salt in beverage; concurrent detection of diphacinone and diphacinone sodium salt samples in positive and negative ion modes is studied by using ion mobility spectrometry technology as basic detection technology and poison detector as detection means. Furthermore, diphacinone sodium salt in beverage, such as coffee, coke and apple juice, can be directly detected without any complicated sample pre-treatment. The measuring method is simple, rapid and reliable. The measuring time only needs 0.5 minutes; and limits of detections can reach 50 ppb respectively. The minimum detection quantity of the diphacinone sodium salt in different beverages is about 1 ng, while 0.06-0.25 g diphacinone sodium salt can cause poisoning when taken by the adults orally, so the quantity can be accurately detected by an ion mobility spectrometry poison detector. Based on application research demand in the aspect of forensic science, a software controller can implement alarm mode according to the poison detection signal.
Description
Technical field
The present invention relates to the detection method of diphacinone and diphacinone-Na, specifically a kind of new fast, sensitive, need not the detection diphacinone of any pre-treatment and the method for diphacinone-Na.This method utilizes poisonous substance fast detecting instrument as analysis means based on the ion mobility spectrometry technology, and detectability can reach 50ppb.This methods analyst speed is fast, only needs 0.5min.Test operation is simple, need not any sample pre-treatments experiment, need not special professional background personnel operation.
Background technology
Diphacinone molecular formula: C
23H
16O
3Molecular mass: 340.36; Chinese: 2-(2,2-diphenyl acetyl group)-1, the 3-indandione; English name: diphacinone; 2-diphenyl acetyl-1,3-indandione; Character description: pale yellow powder, nothing is smelt tasteless, is dissolved in alcohol, acetone and boiling water, is insoluble to benzene and toluene, non-corrosiveness, good stability, long term storage is never degenerated.Fusing point 146-147 ℃.Its sodium salt (often claiming diphacinone-Na) solubleness in 100 ℃ of water is 5%, becomes redness by yellow when being heated to 207-208 ℃, 325 ℃ of decomposition.
Diphacinone is chronic rat poison, is one of present most widely used first generation anti-coagulant rodenticide kind, has good palatability, slow, the good effectiveness of effect.The mode of bait of being suitable on a small quantity, repeatedly poisoning is prevented and treated bandicoot.Dead mouse generally appearred after dispensing in 4-6 days, and the individual no violent malaise symptoms of poisoning.Therefore, be difficult for causing similar vigilance.The absolute majority individuality can be eaten enough is enough to the amount that causes death, and it is more thorough to kill mouse.
The former powder of diphacinone-Na is generally based on preparation poison bait control bandicoot.Active constituent content is 0.025%-0.1% in the poison bait, and concentration is low, good palatability.The general saturated bait throwing in of adopting low concentration, high bait amount, perhaps low concentration, little bait amount, the mode of bait throwing in repeatedly.Use the mode of a capacity bait throwing in, also obtain effect preferably.
Diphacinone and diphacinone-Na all have severe toxicity to people and animals.Become human oral diphacinone-Na 0.06-0.25 gram can cause poisoning, 0.5~2.5 gram can cause death.The fact of diphacinone and diphacinone-Na slow poisoning is subjected to forensic science field (crime of poisoning) and Food Science field (the vegetable poisoning thing is residual) gradually and pays close attention to.At present, the detection method of diphacinone and diphacinone-Na poisonous substance has the high performance liquid chromatography of use, the gentle spectrum-mass spectrometric hyphenated technique of gas chromatography, but because the shortcoming of these technology itself, causing can not direct fast at the scene analyzing and testing.
Ion mobility spectrometry (Ion Mobility Spectrometry, IMS) a kind of separation detection technology that occurs the seventies 20th century of technology is compared with traditional mass spectrum, chromatographic apparatus, has simple in structurely, highly sensitive, and analysis speed is fast, the characteristics of reliable results.Can in atmospheric environment, detect, be suitable for on-the-spot the use micro substance.Therefore this technology can be applied to the online detection of precursor chemicals.Ion mobility spectrometry mainly is made up of chamber, ion gate, drift region and detecting device.Sample gas produces molion in chamber ionization.Ion enters the drift region by the ion gate of periodically opening under the ordering about of electric field.With the continuous striking process of neutral drift gas molecule of adverse current in because these ions migration rate difference separately in electric field makes that different ions obtains separating, it is detected successively to arrive collector.Therefore just can determine the existence of evaluating objects material by transit time, and application peak area or peak height can be determined the concentration of respective substance.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing diphacinone and diphacinone-Na in the ion mobility spectrometry poisonous substance detector fast detecting beverage.
In order to realize direct, quick, the sensitive detection of diphacinone and diphacinone-Na in the beverage, the technical solution used in the present invention is:
The method of diphacinone or diphacinone-Na in a kind of fast detecting beverage, 1) qualitative analysis test: 1-50 μ L diphacinone or diphacinone-Na standard items are dissolved in organic solvent, be made into the solution of 1-100ppm, drip on the sample introduction thin slice, sampling place of ion mobility spectrometry sampled point correspondence position, again the sample introduction thin slice being inserted into pyrolysis analyses in the injector, under positive ion and two kinds of patterns of negative ion, be detecting instrument then, carry out analyzing and testing, obtain detection signal respectively through ionic migration spectrometer with the ionic migration spectrometer; Determine the appearance time of diphacinone under two kinds of patterns of positive ion or negative ion or diphacinone-Na, find that relatively negative ion mode is more suitable for detecting diphacinone or diphacinone-Na;
2) drip to 1-50 μ L beverage on the sample introduction thin slice, sampling place of ion mobility spectrometry sampled point correspondence position, again the sample introduction thin slice being inserted into pyrolysis analyses in the injector, under negative ion mode, be detecting instrument then with the ionic migration spectrometer, carry out analyzing and testing through ionic migration spectrometer, obtain detection signal; In the appearance time contrast of negative ion mode and then definite beverage, whether contain diphacinone or diphacinone-Na according to diphacinone or diphacinone-Na in the appearance time of its acquisition and the last step 1).
Two kinds of patterns of ion mobility spectrometry can detect, but negative ion mode ion mobility spectrometry detection signal is stronger, so the analysis of diphacinone-Na is finished by the ion mobility spectrometry of negative ion mode in the beverage.This method detection speed is fast, need not sample pretreatment process, and Measuring Time is only wanted 0.5min, and is highly sensitive, and detectability can reach 50ppb, and concentration conversion becomes quality to be about 1ng.
In the qualitative analysis test, the solvent of dissolving diphacinone and diphacinone-Na is methyl alcohol, acetone, ethanol or water; Described beverage is coffee, cola, tea or fruit juice, need not other pre-treating method, can directly detect or heat to steam and remove the laggard sample detection of moisture.
The sample introduction thin slice is special-purpose sampling paper, tetrafluoro sheet, sheet metal or the high temperature resistant sampling cloth of teflon.
The preparation of diphacinone and diphacinone-Na solution in the beverage is to be solvent (coffee, cola, cider) with the beverage.
The wherein detection of diphacinone and diphacinone-Na in the beverage, need not to carry out the complex sample pre-treatment, directly get a certain concentration drink soln 1-50 μ L, directly enter ion mobility spectrometry and carry out analyzing and testing, or use well heater to go into ion mobility spectrometry except that moisture is laggard and carry out analyzing and testing 100-105 ℃ of steaming.Wherein diphacinone is difficult to dissolving in beverage, and diphacinone-Na is solubilized in beverage.So relating to the detection of beverage toxicity concentration is that example is analyzed with the diphacinone-Na.
Method provided by the invention fast effective (no complicated sample pre-treatment), applicability is wide, can directly apply to the field quick detection of poisoning.
Advantage of the present invention is as follows:
1. compare with traditional gas chromatography, liquid phase chromatogram-mass spectrometry combination method, the means of ion mobility spectrometry as diphacinone and diphacinone-Na in the analysis beverage are had the following advantages: the whole instrument total amount is easy to carry less than 15kg, the instrument independent operating, do not need computer and external source of the gas and liquid, be fit to on-the-spot the use, the instrument volume is small and exquisite portable; Measuring speed is fast; Do not have complicated sample pre-treatment test, be fit to very much on-site quick screening; The operating cost of instrument is very low, and consumables seldom; The cost performance height of instrument, analysis speed is than fast 10 times of HPLC-UV and GC-MS etc.
2. this measuring method is easy, quick, good reliability.Measuring Time only needs 0.5min, does not have the complex sample pre-treatment, can finish single sample in the 1min and detect, and detectability can reach 50ppb.Based on the applied research demand of forensic science aspect, the software control instrument can be provided with alarm mode according to the poisonous substance detection signal.
Description of drawings
Fig. 1 is for detecting the ion mobility spectrometry structural principle synoptic diagram of diphacinone and diphacinone-Na;
Ionic migration spectrometer adopts traditional uniform field migration spectrum, its structural representation such as Fig. 1.This instrument mainly comprises following components: sampling device 1, ionization source 2, reaction zone 3, ion gate 4, migration tube 5, make-up gas? 6 and signal receive and detection system 7,8,9,10.Wherein, 7 is Faraday cylinder, and 8 is amplifier, and 9 is A/D converter, and 10 is data handling system, and 11 is pressurized air.Sampling device mainly is made up of hot parser, sample introduction thin slice and carrier gas transfer pipeline, and wherein hot parser then mainly is made up of injection port, heating rod and temperature controller.
Fig. 2 is respectively the ion mobility spectrometry figure that detects diphacinone and diphacinone-Na with the negative ion mode ion mobility spectrometry;
Fig. 3 is respectively the ion mobility spectrometry figure that detects diphacinone and diphacinone-Na with the positive ion mode ion mobility spectrometry;
Fig. 4 is for directly detecting the ion mobility spectrometry figure of diphacinone-Na in the coffee with the negative ion mode ion mobility spectrometry;
Fig. 5 is for directly detecting the ion mobility spectrometry figure of diphacinone-Na in the cola with the negative ion mode ion mobility spectrometry;
Fig. 6 is for directly detecting the ion mobility spectrometry figure of diphacinone-Na in the cider with the negative ion mode ion mobility spectrometry.
Embodiment
Described ionic migration spectrometer: with the ionization source is radioactivity
63The Ni source, ultraviolet light ionization source and discharge ionization source.Described ionic migration spectrometer mainly comprises sampling device, ionization source, reaction zone, ion gate, migration area, signal reception and detection system and gas circuit drying system.Sampling device mainly comprises hot parser, sample introduction thin slice and carrier gas transfer pipeline.Wherein hot parser mainly is made up of injection port, heating rod or heating tape, temperature controller, the sample introduction thin slice can be sampling paper, metal grid mesh, poly-tetrafluoro sheet or the special-purpose sampling of teflon cloth, the carrier gas transfer pipeline is made up of four fluorine tube or metal tube and flowmeter, as Fig. 1.
In order to realize quick, the Sensitive Detection of diphacinone and diphacinone-Na, the present invention uses ion mobility spectrometry as analysis means, diphacinone and diphacinone-Na standard items are dissolved in the organic solvent (are made into the solution of 1-100ppm), drip on the sampling paper, under positive and negative two kinds of patterns, be detecting instrument then, obtain detection signal respectively with the ionic migration spectrometer.Wherein the positive ion mode background signal is not as negative ion mode ion mobility spectrometry (as Fig. 2), so the diphacinone in the subsequent experimental beverage and diphacinone-Na analysis are finished by the negative ion mode ion mobility spectrometry.The preparation of diphacinone and diphacinone-Na solution in the beverage is to be solvent (coffee, cola, fruit juice, tea) with the beverage.The detection of this method is limited to 50ppb (3 times of noise signal intensity are defined as minimum detectable level).
Fig. 2-7 has provided some experiment spectrograms the present invention has been given and explanation.The experiment condition of these spectrograms is: the migration tube temperature remains on about 100 ℃ during experiment, and the injector temperature remains on about 180 ℃.
Embodiment 1
Utilize the process of ionic migration spectrometer detection diphacinone and diphacinone-Na methanol solution as follows: the sample solution that extracts 1-50 μ L drops on the sampling thin slice, volatilizes methyl alcohol (80 ℃ of well heaters), inserts the injection port of instrument then.Sample is vaporized fast by a built-in hot parser, and the temperature of hot parser is about 180 ℃; Pyrolysis is analysed the sample gas that obtains and is brought into the ionized region of ion mobility spectrometry by carrier gas, and the flow of carrier gas is about 300sccm; Sample is ionized to negative ions at ionized region, and the ion gate by periodically opening enters the drift region that is made of uniform electric field, obtains in the drift region separating and detects.
Fig. 2 has provided the ion mobility spectrometry figure that detects diphacinone and diphacinone-Na with the negative ion mode ionic migration spectrometer, as can be seen from the figure, negative ion mode reagent ion peak (RIP) appears at about 6.5ms, the appearance time of diphacinone is about 13ms shown in Fig. 2 (a), and the appearance time of diphacinone-Na is about 10.3ms shown in Fig. 2 (b).
Fig. 3 has provided the ion mobility spectrometry figure that detects diphacinone and diphacinone-Na with the positive ion mode ionic migration spectrometer, as can be seen from the figure, (RIP) appears at about 4.5ms at the reagent ion peak, the appearance time of diphacinone is about 8.8ms shown in Fig. 3 (a), and the appearance time of diphacinone-Na is about 7.0ms shown in Fig. 3 (b).
Utilize the process of diphacinone-Na in the ionic migration spectrometer detection beverage as follows: the sample solution that extracts 1-50 μ L drops on the clean sampling thin slice, inserts the injection port of instrument then.Sample is vaporized fast by a built-in hot parser, and the temperature of hot parser is about 180 ℃; Pyrolysis is analysed the sample gas that obtains and is brought into the ionized region of ion mobility spectrometry by carrier gas, and the flow of carrier gas is about 300sccm; Sample is ionized to negative ions at ionized region, and the ion gate by the cycle opens enters the drift region that is made of uniform electric field, obtains in the drift region separating and detects.The mobility constant of different compounds is variant, the speed difference that moves in the drift region, and they arrive the asynchronism(-nization) of detecting device.Measure time and peak intensity that ion arrives detector, just can confirm classes of compounds, and according to its content of signal strength measurement at peak.
That Fig. 4 provides is the ion mobility spectrometry figure that the negative ion mode ion mobility spectrometry directly detects diphacinone-Na in the coffee; Diphacinone-Na is well detected in the coffee, and reagent ion peak (RIP) appears at about 6.5ms, and the characteristic peak of diphacinone-Na is at 10.3ms.Other composition in the coffee has detecting signal simultaneously, but does not disturb the detection of diphacinone-Na, detects and is limited to 50ppb.
That Fig. 5 provides is the ion mobility spectrometry figure that the negative ion mode ion mobility spectrometry directly detects diphacinone-Na in the cola; Diphacinone-Na is well detected in the cola, and reagent ion peak (RIP) appears at about 6.5ms, and the characteristic peak of diphacinone-Na is at 10.3ms.Other composition in the cola has detecting signal simultaneously, but does not disturb the detection of diphacinone-Na, detects and is limited to 50ppb.
That Fig. 6 provides is the ion mobility spectrometry figure that the negative ion mode ion mobility spectrometry directly detects diphacinone-Na in the cider; Diphacinone-Na is well detected in the cider, and reagent ion peak (RIP) appears at about 6.5ms, and the characteristic peak of diphacinone-Na is at 10.3ms.Other composition in the cider has detecting signal simultaneously, but does not disturb the detection of diphacinone-Na, detects and is limited to 50ppb.
Claims (6)
1. the method for diphacinone or diphacinone-Na in the fast detecting beverage is characterized in that:
1) qualitative analysis test: diphacinone or diphacinone-Na standard items are dissolved in organic solvent, be made into the solution of 1-100ppm, get that 1-50 μ L drips on the sample introduction thin slice, sampling place of ion mobility spectrometry sampled point correspondence position, again the sample introduction thin slice being inserted into pyrolysis analyses in the injector, under positive ion and two kinds of patterns of negative ion, be detecting instrument then with the ionic migration spectrometer, carry out analyzing and testing through ionic migration spectrometer, obtain detection signal respectively; Determine the appearance time of diphacinone under two kinds of patterns of positive ion or negative ion or diphacinone-Na;
2) drink sample analytical test: with 1-50 μ L beverage drip on the sample introduction thin slice, sampling place of ion mobility spectrometry sampled point correspondence position, again the sample introduction thin slice being inserted into pyrolysis analyses in the injector, under positive ion or negative ion mode, be detecting instrument then with the ionic migration spectrometer, carry out analyzing and testing through ionic migration spectrometer, obtain detection signal; According to whether containing diphacinone or diphacinone-Na in the appearance time contrast of the appearance time of its acquisition and diphacinone in the last step 1) or diphacinone-Na and then the definite beverage.
2. method according to claim 1 is characterized in that: in the qualitative analysis test, the solvent of dissolving diphacinone and diphacinone-Na is methyl alcohol, acetone, ethanol or water.
3. method according to claim 1 is characterized in that: described beverage is coffee, cola, tea or fruit juice, need not sample-pretreating method, but direct injected detects or heating is steamed except that the laggard sample detection of moisture.
4. method according to claim 1 is characterized in that: described check and analysis are finished by the ion mobility spectrometry of negative ion mode.
5. method according to claim 1 is characterized in that: described detectability can reach 50ppb.
6. method according to claim 1 is characterized in that: the sample introduction thin slice is special-purpose sampling paper, tetrafluoro thin slice, sheet metal or the high temperature resistant sampling cloth of teflon.
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Cited By (6)
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CN103884768A (en) * | 2012-12-21 | 2014-06-25 | 中国科学院大连化学物理研究所 | Method for rapidly analyzing saliva poisons |
CN104031887A (en) * | 2014-03-19 | 2014-09-10 | 中国农业大学 | Monoclonal antibody and application thereof in diphacinone detection |
CN104111284A (en) * | 2013-04-18 | 2014-10-22 | 中国科学院大连化学物理研究所 | Method for rapidly sensitively detecting sodium valproate in blood |
CN104777160A (en) * | 2015-03-27 | 2015-07-15 | 浙江大学 | Method for rapidly detecting diphacinone sodium salt, and detection kit thereof |
CN105510113A (en) * | 2014-09-25 | 2016-04-20 | 中国科学院大连化学物理研究所 | Method for improving thermal desorption efficiency of to-be-detected sample |
CN106841367A (en) * | 2015-12-07 | 2017-06-13 | 中国科学院大连化学物理研究所 | A kind of Ion transfer spectrum detection method of time resolution Dynamic Thermal parsing |
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Cited By (8)
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CN103884768A (en) * | 2012-12-21 | 2014-06-25 | 中国科学院大连化学物理研究所 | Method for rapidly analyzing saliva poisons |
CN104111284A (en) * | 2013-04-18 | 2014-10-22 | 中国科学院大连化学物理研究所 | Method for rapidly sensitively detecting sodium valproate in blood |
CN104031887A (en) * | 2014-03-19 | 2014-09-10 | 中国农业大学 | Monoclonal antibody and application thereof in diphacinone detection |
CN104031887B (en) * | 2014-03-19 | 2016-05-25 | 中国农业大学 | A kind of monoclonal antibody and the application in detection diphacinone thereof |
CN105510113A (en) * | 2014-09-25 | 2016-04-20 | 中国科学院大连化学物理研究所 | Method for improving thermal desorption efficiency of to-be-detected sample |
CN104777160A (en) * | 2015-03-27 | 2015-07-15 | 浙江大学 | Method for rapidly detecting diphacinone sodium salt, and detection kit thereof |
CN104777160B (en) * | 2015-03-27 | 2018-08-17 | 浙江大学 | A kind of method and its detection kit that diphacinone-Na quickly detects |
CN106841367A (en) * | 2015-12-07 | 2017-06-13 | 中国科学院大连化学物理研究所 | A kind of Ion transfer spectrum detection method of time resolution Dynamic Thermal parsing |
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Application publication date: 20111228 |