CN107607489A - A kind of paraquat quick determination method and its detection means - Google Patents
A kind of paraquat quick determination method and its detection means Download PDFInfo
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- CN107607489A CN107607489A CN201710668598.5A CN201710668598A CN107607489A CN 107607489 A CN107607489 A CN 107607489A CN 201710668598 A CN201710668598 A CN 201710668598A CN 107607489 A CN107607489 A CN 107607489A
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Abstract
The invention discloses a kind of detection method based on Rayleigh resonance light scattering principle quantitative determination paraquat content, belong to Physico-chemical tests field.The detection method includes sample obtaining step, pre-treatment step, sequentially adds three kinds of reagent steps, measuring process and result step display.The invention also discloses a kind of portable instrumentation using above-mentioned detection method, the detecting instrument includes measurement bottle fixed support, tungsten light source, Amici prism, light splitting slit, light-splitting processing unit, signal processing unit, display unit, sample vacuum desiccator, the first reagent box support, the second reagent box support, the 3rd reagent box support and standard reagent box support.The present invention is adapted to the quick detection of the paraquat content of a variety of different samples.
Description
Technical field
The present invention relates to Physico-chemical tests field, more particularly to a kind of for paraquat fast qualitative, the dress of quantitative determination
Put and detection method.
Background technology
Paraquat is a kind of efficient, widely used herbicide.Because it is using extensive, it is annual have much wrongly take, commit suiside,
Excessively contact and cause the event of acute poisoning to occur, because clinically there is no effective antidote, paraquat poisoning is lethal
Rate is higher.Carry out the measure that many methods are used for paraquat in biological specimen at present, including:Ultraviolet spectrophotometry,
EUSA, gas chromatography, liquid chromatography, liquid chromatograph mass spectrography, capillary immunoassay etc..
Due to low quality concentration level of the paraquat in urine and the interference of complicated bio-matrix, existing detection method needs large-scale plant
Equipment, analyze speed are slow, it is impossible to realize the quick detection purpose required by clinical economics and basic unit's popularization and application.
In addition, existing detection method is confined to carry out paraquat detection for a certain certain types of sample more, its
Detection reagent is suitable only for the particular type sample.Many aspects are likely to occur in for paraquat poisoning scene, are generally related to
And there is certain limitation in the present situation of a variety of testing samples, existing detection method.
In order to improve the clinical diagnosis speed of the treatment of doubtful paraquat poisoning, for the sample detection under different scenes,
Be easy to promote and use in basic medical unit simultaneously, be badly in need of it is a kind of can fast qualitative, quantitatively to detect different sample paraquats dense
The apparatus and method of degree.Inventor is carried by studying the detection method of paraquat, characteristic and the general principle of Rayleigh resonance scattering
Apparatus and method of the present invention are gone out.
The content of the invention
In order to quick and precisely detect the paraquat content in different type sample, the present invention provides one kind and is based on Rayleigh
The detection method of resonance light scattering principle quantitative determination paraquat content, the detection method include sample obtaining step, pre-
Processing step, sequentially add three kinds of reagent steps, measuring process and result step display.
In the sample obtaining step, including acquisition water to be measured, urine to be measured, test plasma, fruits and vegetables sample to be measured extremely
A kind of few sample;
Further, it is as follows for the sample obtaining step difference of water, urine, blood plasma, fruits and vegetables:
(1) the 2ml water or urine sample of paraquat may be contained by obtaining, through the water-based filtering with microporous membrane of 0.22um in PP samples
Guan Zhong;
(2) the 1ml plasma samples of paraquat may be contained by obtaining, and 4ml acetonitrile precipitation albumen is added dropwise under vortex oscillation,
10000g centrifuges 2min, and 2ml supernatants are transferred in PP sample cells;
(3) the 5g vegetables and fruits class samples of paraquat may be contained by obtaining, and added 5ml water and smashed to pieces, be vortexed vibration 2min, 10000g from
Heart 2min, after supernatant liquid decolourizes, aqueous phase is transferred in PP sample cells.
The pre-treatment step, including the sample to being obtained in the sample acquisition step pre-process, and will locate in advance
Sample after reason is transferred in PP sample cells;
It is described to sequentially add three kinds of reagent steps, including:The PP sample cells are placed in vacuum desiccator, carry out 50 DEG C
Drying concentration under condition of negative pressure, 1 the first kit reagent is then added, be transferred to after shaking up in measurement bottle;Again plus
Enter 1 the second kit reagent, shake up 2~3 times, be eventually adding 1 the 3rd kit reagent, after covering tightly sample bottle cap, slowly
It is reverse to shake up 2~3 times, stand 10~30min;
The measuring process includes:The measurement bottle is positioned over to the measurement bottle fixed support position of paraquat detection means
Upper progress paraquat content detection;
The result step display includes:The paraquat of real-time display testing sample contains on the display screen of detection means
Amount;
First kit is that glass pacifies general bottle, and glass pacifies the acetic acid that general bottle prepackage 1ml concentration is 50mmol/L concentration
Ammonium cushioning liquid, the μ l containing acetic acid 10 in the ammonium acetate buffer solution;In use, every part of sample pacifies general bottle using 1 glass
Buffer solution;Second kit is preinstalled with 1ml Nessler's reagents, and second kit is that glass pacifies general bottle, and glass pacifies general bottle
It is 50mmol/L concentration Nessler's reagents to pre-install 1ml concentration, in use, every part of sample pacifies the buffer solution of general bottle using 1 glass;
3rd kit is preinstalled with 1ml dispersants, and the 3rd kit is that glass pacifies general bottle, and glass is pacified general bottle prepackage 1ml and told
Temperature -100, in use, every part of sample pacifies the dispersant of general bottle using 1 glass.
Large-scale plant equipment is needed for existing detection method, analyze speed is slow, it is impossible to required by realizing clinical economics
Quick detection purpose and the problem of basic unit's popularization and application, the invention also discloses one kind to utilize above-mentioned detection method fast quantification
Determine the portable detector of paraquat content.
All parts of the device use integrated manufacture, portable carrying;Do not limited by use environment.
Specifically, the detection means includes measurement bottle fixed support, tungsten light source, Amici prism, light splitting slit, light splitting
Processing unit, signal processing unit and display unit;Also include:
Sample vacuum desiccator, the first reagent box support, the second reagent box support, the 3rd kit and rack standard reagent
Box support;
Wherein,
On the left of light splitting slit, measurement bottle is in light path on the right side of light splitting slit for tungsten light source and Amici prism
Center, light-splitting processing unit turn 90 degrees position partially in incident light luminosity, and is connected to signal processing unit, signal transacting list
Member is connected with display screen;
The light-splitting processing unit includes photomultiplier, and the light-splitting processing unit receives what is sent from tungsten light source
From the light that light splitting slit is incident after Amici prism is handled, electric signal is translated into;
The signal processing unit includes A/D converter and processor, and the electric signal is converted into data signal by it, and
The concentration of paraquat in testing sample is calculated by processor, and shows on the display unit;The measurement bottle fixes branch
Frame, tungsten light source, Amici prism, light splitting slit, light-splitting processing unit, signal processing unit, display unit, sample vacuum drying
Device, the first reagent box support, the second reagent box support, the 3rd reagent box support and standard reagent box support are integrated.
For different testing samples, after obtaining testing sample and being pre-processed, sample enters measurement bottle, then will survey
Measuring bottle is placed on the measurement bottle fixed support of described device and can detected;Meanwhile detect the first to the 3rd reagent of use
And standard reagent can be placed on, the first reagent box support, the second reagent box support, the 3rd reagent with pre-configured
On box support and standard reagent box support, according to sample pretreatment and detection needs, add on demand, it is convenient and swift.
The invention can be used for the fast qualitative of paraquat in water, urine, blood, soil, vegetables and fruits class medium, quantitative inspection
Survey, the clinical diagnosis for doubtful paraquat poisoning provides effective detection.The invention and existing Technical comparing, there is detection speed
Degree, applicability are wide, simple to operate, without large-scale experiment room detection means, the characteristics of limitation by use environment.
Brief description of the drawings
Fig. 1 is the detection method based on Rayleigh resonance light scattering principle quantitative determination paraquat content of the present invention
Step schematic diagram.
Fig. 2 is the schematic diagram of the detection means of the present invention.
Embodiment
For specific explanations technical scheme, illustrated by specific examples below.
As shown in Fig. 2 a kind of portable detector of quantitative determination paraquat content, including measurement bottle fix branch
Frame, tungsten light source, Amici prism, light splitting slit, light-splitting processing unit, signal processing unit and display unit, sample vacuum are done
Dry device, the first reagent box support, the second reagent box support, the 3rd kit and rack standard reagent box support;Wherein, tungsten lamp light
Source and Amici prism are on the left of light splitting slit, and measurement bottle is in optical path Center position on the right side of light splitting slit, at light splitting
Reason unit turn 90 degrees position partially in incident light luminosity, and is connected to signal processing unit, and signal processing unit is connected with display screen;
The light-splitting processing unit includes photomultiplier, and the light-splitting processing unit receives what is sent from tungsten light source
From the light that light splitting slit is incident after Amici prism is handled, electric signal is translated into;
The signal processing unit includes A/D converter and processor, and the electric signal is converted into data signal by it, and
The concentration of paraquat in testing sample is calculated by processor, and shows on the display unit;The measurement bottle fixes branch
Frame, tungsten light source, Amici prism, light splitting slit, light-splitting processing unit, signal processing unit, display unit, sample vacuum drying
Device, the first reagent box support, the second reagent box support, the 3rd reagent box support and standard reagent box support are integrated.
According to Beer-Lambert Law, light path, incident intensity and wavelength it is certain under conditions of, the intensity of Rayleigh scattering light
It is linear within the specific limits with the concentration of testing sample, meet Lambert-Beer's law, can be obtained by standard liquid
The content of paraquat in once linear regression equation calculation testing sample solution, it can be calculated further according to sample volume (quality) to be measured
The concentration of paraquat in sample.
For different testing samples, after obtaining testing sample and being pre-processed, sample enters measurement bottle, then will survey
Measuring bottle is placed on the measurement bottle fixed support of described device and can carry out being detected and being examined according to the method described in accompanying drawing 1
Survey result.
Compared with the prior art, product of the present invention has advantages below and effect:
(1) it is easy to configure and use in basic medical unit;
(2) simple to operate, analyze speed is fast, and the clinical economics available for doubtful paraquat patients with acute intoxication quickly sieve
Look into;Effect is directly perceived;
(3) use cost is low, without large scale equipment;Can field use, do not limited by place
(4) different types of testing sample is applicable to, and detection reagent can update replacement.
Claims (10)
1. a kind of detection method based on Rayleigh resonance light scattering principle quantitative determination paraquat content, the detection method bag
Include sample obtaining step, pre-treatment step, sequentially add three kinds of reagent steps, measuring process and result step display, it is special
Sign is:
At least one in the sample obtaining step, including acquisition water to be measured, urine to be measured, test plasma, fruits and vegetables sample to be measured
Kind sample;
The pre-treatment step, including the sample to being obtained in the sample acquisition step pre-process, and by after pretreatment
Sample be transferred in PP sample cells;
It is described to sequentially add three kinds of reagent steps, including:
The PP sample cells are placed in vacuum desiccator, the drying concentration under 50 DEG C of condition of negative pressure is carried out, then adds 1
The first kit reagent of branch, it is transferred to after shaking up in measurement bottle;1 the second kit reagent is added, shakes up 2~3 times, finally
1 the 3rd kit reagent is added, it is slowly reverse to shake up 2~3 times after covering tightly sample bottle cap, stand 10~30min;
First kit is preinstalled with 1ml buffer solutions, and the second kit is preinstalled with 1ml Nessler's reagents, the prepackage of the 3rd kit
There are 1ml dispersants;
The measuring process includes:
The measurement bottle is positioned over progress paraquat content detection on the measurement bottle fixed support position of paraquat detecting instrument;
The result step display includes:The paraquat content of real-time display testing sample on the display screen of detecting instrument.
2. detection method according to claim 1, first kit is preinstalled with 1ml buffer solutions, it is characterised in that:Institute
To state the first kit and pacify general bottle for glass, glass pacifies the ammonium acetate buffer solution that general bottle prepackage 1ml concentration is 50mmol/L concentration,
The μ l containing acetic acid 10 in the ammonium acetate buffer solution;In use, every part of sample pacifies the buffer solution of general bottle using 1 glass.
3. detection method according to claim 1, second kit is preinstalled with 1ml Nessler's reagents, it is characterised in that:
Second kit is that glass pacifies general bottle, and it is 50mmol/L concentration Nessler's reagents that glass, which pacifies general bottle prepackage 1ml concentration, is used
When, every part of sample pacifies the buffer solution of general bottle using 1 glass.
4. detection method according to claim 1, the 3rd kit is preinstalled with 1ml dispersants, it is characterised in that:Institute
State the 3rd kit and pacify general bottle for glass, glass pacifies general bottle prepackage 1ml tween -100, in use, every part of sample uses 1 glass
Pacify the dispersant of general bottle.
A kind of 5. portable inspection of detection method quantitative determination paraquat content using described in claim any one of 1-4
Survey device, including measurement bottle fixed support, tungsten light source, Amici prism, light splitting slit, light-splitting processing unit, signal transacting list
Member and display unit;Characterized in that, also include:
Sample vacuum desiccator, the first reagent box support, the second reagent box support, the 3rd kit and rack standard kit branch
Frame;Wherein,
On the left of light splitting slit, measurement bottle is in optical path Center on the right side of light splitting slit for tungsten light source and Amici prism
Position, light-splitting processing unit turn 90 degrees position partially in incident light luminosity, and is connected to signal processing unit, signal processing unit with
Display screen connects;
The light-splitting processing unit includes photomultiplier, and the light-splitting processing unit receives the process sent from tungsten light source
From the light that light splitting slit is incident after Amici prism processing, electric signal is translated into;
The signal processing unit includes A/D converter and processor, and the electric signal is converted into data signal by it, and is passed through
The concentration of paraquat in testing sample is calculated in processor, and shows on the display unit;The measurement bottle fixed support, tungsten
Lamp source, Amici prism, light splitting slit, light-splitting processing unit, signal processing unit, display unit, sample vacuum desiccator, the
One reagent box support, the second reagent box support, the 3rd reagent box support and standard reagent box support are integrated.
6. portable detector as claimed in claim 5, wherein, paraquat in testing sample is calculated by processor
Concentration, and show on the display unit, including:The strong of the Rayleigh resonance light scattering of testing sample is shown on the display unit
Degree, the once linear regression equation calculation testing sample solution obtained by the paraquat standard reference material pre-installed in standard reagent box
The content of middle paraquat, further according to the concentration of paraquat in sample volume and/or Mass Calculation testing sample.
7. portable detector as claimed in claim 5, it is characterised in that:Light source used in the tungsten light source includes as follows
One of:(1) high energy halogen tungsten lamp light source;(2) the special halogen bulb of the order of spectrum of the life-span more than 10,000 hours.
8. portable detector as claimed in claim 5, the Amici prism is Single wavelength Amici prism, and its feature exists
In being divided the incident wavelength used and be fixed as 500nm;The light splitting slit is Amici prism and the survey among detection darkroom
Physics light spacer between measuring bottle, it is characterised in that:The light splitting slit is on the aluminium alloy plate of 1mm thickness, and processing is wide
Spend for 100 μm, length is that 10mm narrow window obtains, for obstructing the veiling glare in addition to 500nm wavelength;The detection darkroom
For the shell of whole portable detector, it is characterised in that:After darkroom hatch door is shut, except the light that tungsten light source is sent is by dividing
Obtained after light prismatic decomposition outside the light splitting that wavelength is 500nm, enter the darkroom without any other veiling glare, it is ensured that light-splitting processing list
The accuracy for the incident light that member receives.
9. portable detector as claimed in claim 5, the measurement bottle is the container of sample solution, and its feature exists
In:Sample cell is cylinder, and pool wall is that internal diameter is 5mm, and external diameter is 7mm quartz cylinder optical window, and bottom of pond is high borosilicate glass
Glass.
10. portable detector as claimed in claim 5, the sample vacuum desiccator is sample concentration device, and it is special
Sign is:With heating function, drier bottom for can heat conduction aluminum alloy bottom plate, have 1 circle seal washer, the sealing on bottom plate
Bell polycarbonate cap supports the use above packing ring and drier, and bell lid and bottom plate shape is into good air-tightness, and poly- carbonic acid
Needle valve is separately installed with ester bell cover, vacuumizes interface and vacuum meter.
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