CN108918709A - Screening, quantitative detecting method and the application of common herbicide in a kind of blood - Google Patents
Screening, quantitative detecting method and the application of common herbicide in a kind of blood Download PDFInfo
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- CN108918709A CN108918709A CN201810765866.XA CN201810765866A CN108918709A CN 108918709 A CN108918709 A CN 108918709A CN 201810765866 A CN201810765866 A CN 201810765866A CN 108918709 A CN108918709 A CN 108918709A
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- G01N30/02—Column chromatography
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- G—PHYSICS
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- 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
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Abstract
The present invention relates to the screenings of common herbicide, quantitative detecting method in a kind of blood, it is characterised in that：Pre-treatment is carried out to blood sample with precipitation of protein, detects the herbicide in the blood sample with liquid chromatogram/high resolution mass spectrum combination analysis method.The present invention is after carrying out pre-treatment to blood sample with precipitation of protein, the protein precipitation of interference measurement can be removed, and still reside in herbicide to be measured in blood sample, cooperate liquid chromatogram/high resolution mass spectrum combination analysis method, quickly, easily can extract a variety of herbicides in blood simultaneously.This method can be used for legal medical expert and determine to analyze herbicide type and content in blood sample during Toxicosis Death.
Description
Technical field
The invention belongs to the screenings of common herbicide, quantitative inspection in technical field of biological more particularly to a kind of blood
Survey method.
Background technique
Herbicide is widely used during modern agricultural production, and output and usage amount increase year by year, at present China
Common herbicide includes more than 20 types such as quaternary amine, organic phosphorus, amide, sulfonylureas and three pyridines.However, being drawn by herbicide
Rise Poisoning Cases also increase therewith, in blood herbicide carry out fast and accurately qualitatively screening to quantitative analysis to related case
Part detection is significant.Since herbicide is many kinds of, property multiplicity, sample pre-treatments and instrument analytical method are not quite similar.
The detection method of herbicide mainly has liquid chromatography mass to be combined method, capillary electrophoresis, thin-layer chromatography in biological material at present
Method, gas chromatography, gas chromatography mass spectrometry method and immunoassay etc..In the method for existing literature report, conventional sample pretreatment side
Method such as liquid-liquid extraction and Solid Phase Extraction can only extract certain kin several herbicides from blood, and majority is only fitted
For the detection of single type herbicide, screening is carried out to multiple types herbicide and quantitative detection method is rarely reported, nothing
The needs of method meets while carrying out screening and quantitative detection to multiple types herbicide, therefore can not quickly judge poisoner's blood
In herbicide type and content.
Summary of the invention
For the prior art can only extract single type herbicide from blood, majority is only applicable to single type
Herbicide detection technique problem, the present invention provides the screenings of common herbicide, quantitative detecting method in a kind of blood.
And the present invention also provides the above methods analyzed during determining Toxicosis Death in blood sample herbicide type and
The application of content.
To achieve the above object of the invention, the embodiment of the present invention uses the following technical solution：
The screening of common herbicide, quantitative detecting method, carry out pre-treatment to blood sample with precipitation of protein in a kind of blood,
The herbicide in the blood sample is detected with liquid chromatogram/high resolution mass spectrum combination analysis method.
In terms of existing technologies, the present invention can will be done after carrying out pre-treatment to blood sample with precipitation of protein
The protein precipitation for disturbing measurement removes, and herbicide to be measured is still resided in blood sample, cooperation liquid chromatogram/high resolution mass spectrum connection
With analysis method, can quickly, easily a variety of herbicides in screening blood simultaneously.
Preferably, the concrete operation step of the precipitation of protein is：It is added into the blood sample and is equivalent to the blood sample 4
The protein precipitant of~5 times of volumes, be vortexed 60~90s, after 5~10min of ultrasound, 10000~12000rpm/min centrifugation 10~
15min, take supernatant to get；Wherein, the protein precipitant is 75v/v% acetonitrile solution.The precipitating reagent not with herbicide
It chemically reacts, and not interference measurement, protein precipitation in blood sample can be made complete.
Preferably, in the liquid chromatogram/high resolution mass spectrum combination analysis method, the chromatographic condition of the liquid chromatogram
For：
Chromatographic column：Octadecylsilane chemically bonded silica chromatographic column；
Mobile phase A is 0.1% formic acid solution, and Mobile phase B is methanol, carries out linear gradient elution, the linear elution ladder
It spends as follows：
Flow velocity：0.3mL/min.
Preferred chromatographic column makes and mobile phase makes liquid phase detection method sensitivity with higher, accuracy and reproduction
Property.Such as Hypersil GOLD C-18 chromatographic column, gained chromatographic peak peak shape is sharply symmetrical, and all substances can be kept completely separate,
Noise is relatively high.It is preferred that gradient can make different herbicides have respectively different appearance times, peak shape and separation effect
Fruit is convenient for comparative observation, so as to accurately judge the type and concentration of herbicide in blood sample.When 0.1% first of mobile phase
Acid solution/methanol volume ratio is 95：When 5, separating effect is best, and ionising effects are most strong, sensitivity highest.
Preferably, the analysis condition of the high resolution mass spectrum is：
Ion source：The source HESI；
Electron spray voltage：3200V；
Capillary temperature：320℃；
Auxiliary heater temperature：300℃；
Sheath gas：Nitrogen, flow velocity 30L/min；
Assist gas：Nitrogen, flow velocity 15L/min；
Data scanning mode：The level-one full scan of positive and negative switching/real-time secondary scanning of the mass spectrum mode, the level-one full scan
The resolution ratio of mode is 70000, and the resolution ratio of second level scan pattern is 17500.
The high resolution mass spectrum condition has stronger specificity and higher sensitivity, accuracy and reproducibility, makes to detect
As a result more accurate.
Preferably, the type of the herbicide includes quaternary ammonium salt, organic phosphates, triazine, imidazolone type, amide
Class, sulfonylurea, diphenyl ether, phenoxy carboxylic acid, benzoic acids, aryloxyphenoxypropionic class, dinitroaniline, pyridine
At least one of carboxylic acids and cyclohexenone analog.Above-mentioned herbicide type is herbicide kind common in herbicide intoxication conditions
Class.
Preferably, quaternary ammonium salt herbicide includes at least one of paraquat and diquat dibromide；And/or
Organic phosphates herbicide includes at least one of glyphosate and glufosinate-ammonium；And/or
Triazine herbicide includes at least one of cyanazine, atrazine, Simanex, symetryne and prometryn；With/
Or
Imidazolinone herbicide is imazapyr；And/or
Acetamide-group herbicides include at least one of metazachlor, Acetochlor and propisochlor；And/or
Sulfonylurea herbicide includes at least one of chlorsulfuron, metsulfuron-methyl, bensulfuron-methyl and oxasulfuron；With/
Or
Diphenyl ether herbicide is Bentazon；And/or
Benzene oxycarboxylic acid and benzoic acid herbicide are dicamba；And/or
Aryloxyphenoxypropionic class herbicide includes at least one of haloxyfop-P-methyl and quizalofop-ethyl；And/or
Dinitroaniline herbicide includes at least one of Pendimethalin and Amex820；And/or
Picolinic acid class herbicide is clopyralid；And/or
Cyclohexenone analog herbicide is alloxydimsodium.
And it analyzes in blood sample and removes during legal medical expert determines Toxicosis Death the embodiment of the invention also provides the above method
The application of careless agent type and content.By the above method, it can stablize, quickly and accurately common type in blood sample to be measured is removed
Careless agent carries out qualitatively screening and quantitative analysis, is of great significance for the detection of herbicide poisoning Related Cases.
Detailed description of the invention
Fig. 1 is the extraction chromatography of ions figure of paraquat in embodiment；
Fig. 2 is the extraction chromatography of ions figure of diquat dibromide in embodiment；
Fig. 3 is the extraction chromatography of ions figure of embodiment glyphosate；
Fig. 4 is the extraction chromatography of ions figure of glufosinate-ammonium in embodiment；
Fig. 5 is the extraction chromatography of ions figure of cyanazine in embodiment；
Fig. 6 is the extraction chromatography of ions figure of atrazine in embodiment；
Fig. 7 is the extraction chromatography of ions figure of Simanex in embodiment；
Fig. 8 is the extraction chromatography of ions figure of symetryne in embodiment；
Fig. 9 is the extraction chromatography of ions figure of prometryn in embodiment；
Figure 10 is the extraction chromatography of ions figure of imazapyr in embodiment；
Figure 11 is the extraction chromatography of ions figure of metazachlor in embodiment；
Figure 12 is the extraction chromatography of ions figure of Acetochlor in embodiment；
Figure 13 is the extraction chromatography of ions figure of propisochlor in embodiment；
Figure 14 is the extraction chromatography of ions figure of chlorsulfuron in embodiment；
Figure 15 is the extraction chromatography of ions figure of metsulfuron-methyl in embodiment；
Figure 16 is the extraction chromatography of ions figure of bensulfuron-methyl in embodiment；
Figure 17 is the extraction chromatography of ions figure of oxasulfuron in embodiment；
Figure 18 is the extraction chromatography of ions figure of Bentazon in embodiment；
Figure 19 is the extraction chromatography of ions figure of dicamba in embodiment；
Figure 20 is the extraction chromatography of ions figure of haloxyfop-P-methyl in embodiment；
Figure 21 is the extraction chromatography of ions figure of quizalofop-ethyl in embodiment；
Figure 22 is the extraction chromatography of ions figure of Pendimethalin in embodiment；
Figure 23 is the extraction chromatography of ions figure of Amex820 in embodiment；
Figure 24 is the extraction chromatography of ions figure of clopyralid in embodiment；
Figure 25 is the extraction chromatography of ions figure of alloxydimsodium in embodiment.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.
Embodiment 1
It is specific as follows the embodiment of the invention provides the screening of common herbicide, quantitative detecting method in a kind of blood：
1. reagent
Paraquat, diquat dibromide, glyphosate, glufosinate-ammonium, cyanazine, atrazine, Simanex, symetryne, prometryn, imidazoles cigarette
Acid, metazachlor, Acetochlor, propisochlor, chlorsulfuron, metsulfuron-methyl, bensulfuron-methyl, oxasulfuron, Bentazon, dicamba, fluorine
Shanghai City pesticide research is purchased from than the spirit of first standing grain, Kui Heling, Pendimethalin, Amex820, clopyralid, alloxydimsodium standard items
Co., Ltd of institute is the water or methanol standard solution of concentration 1mg/ml.Acetonitrile, methanol (chromatographically pure) are purchased from U.S. Thermo
Fisher company, formic acid (chromatographically pure) are purchased from U.S. DIKMA company, and experimental water is the Milli-Q system (U.S.
Millipore company) preparation ultrapure water.
2. instrument
Thermo ScientificTM Q ExactiveTMFocus ultrahigh pressure liquid phase chromatography-high resolution mass spec combination
Instrument (Thermo Fisher company of the U.S.), high speed freezing centrifuge (Thermo Fisher company of the U.S.), vortex oscillator (beauty
CORNING company of state), KQ-500DE type numerical control ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.).
3. solution is prepared
Hybrid standard reserve supply liquid：The accurate above-mentioned each standard solution of 50 μ L of drawing uses purified water in same volumetric flask
It is settled to 10mL, the hybrid standard reserve supply liquid that each standard items mass concentration is 5 μ g/mL is obtained, is stored in 4 DEG C of refrigerators
It is spare.
Hybrid standard substance working solution：5 μ g/mL hybrid standard reserve supply liquid are taken, are prepared after being diluted step by step with mobile phase
At each standard items mass concentration be respectively 4000ng/mL, 3000ng/mL, 2000ng/mL, 1000ng/mL, 500ng/mL,
The hybrid standard substance working solution of 100ng/mL, 50ng/mL, 20ng/mL, 10ng/mL, 5ng/mL, 1ng/mL, 0.5ng/mL.
Mobile phase：Mobile phase A：2mL formic acid is diluted to 2000mL with ultrapure water, obtains 0.1% formic acid solution；Mobile phase
B：Pure methanol.
Protein precipitant：Acetonitrile/water (3: 1, v/v).
4. sample pre-treatments
It is divided into 12 parts with blood to experiment, is separately added into above-mentioned hybrid standard substance working solution, obtains containing various concentration
The mark-on blood of titer.Each 200 μ L of mark-on blood is taken, acetonitrile/water (3 is separately added into：1, v/v) 800 μ L of mixed solvent is vortexed
After 1min, ultrasonic 5min, 12000r/min protein precipitation by centrifugation 10min carries out liquid phase color after taking supernatant to cross 0.2 μm of filter membrane
Spectrum/high resolution mass spectrum combination analysis.
5. liquid chromatogram and high resolution mass spectrum condition
5.1 high resolution liquid chromatography conditions：
Chromatographic column：Security Guard C-18 pre-column (10 × 4mm, 3 μm, Thermo Fisher company of the U.S.),
Hypersil GOLD C-18 chromatographic column (100 × 2.1mm, 1.9 μm, Thermo Fisher company of the U.S.).
Column temperature：Room temperature.
Using linear elution, gradient is as follows：
Flow velocity：0.3mL/min, sample volume are 1 μ L.
The chromatogram of each herbicide is as shown in Figure 1.
5.2 high resolution mass spectrum analysis conditions are：
Ion source：The source HESI；
Electron spray voltage：3200V；
Capillary temperature：320℃；
Auxiliary heater temperature：300℃；
Sheath gas：Nitrogen, flow velocity 30L/min；
Assist gas：Nitrogen, flow velocity 15L/min；
Data scanning mode：The full scan of positive and negative switching/real-time secondary scanning of the mass spectrum (Full MS/dd-MS2) mode, one
The resolution ratio of grade full scan mode (50-750) is 70000, the resolution ratio 17500 of second level scan pattern (dd-MS2).
By continuous Injection Analysis concentration be 1 μ g/mL single standard items, detect each object precursor and second level from
Son, the mass spectrometry parameters and extraction chromatography of ions figure of detection the results are shown in Table 1.
6. methodological study
6.1 linear relationships and detection limit
Hybrid standard substance working solution mixed standard solution is measured under conditions of 5.1 and 5.2, with quota ion
Pair peak area to mass concentration draw linear relationship curve.The result shows that each herbicide linear relationship in surveyed range is good
It is good, related coefficient (R2) it is all larger than 0.995.Detection limit (LOD) is within the scope of 0.5~50ng/ml, equation of linear regression, phase
Relationship number and detection limit are shown in Table 2.
Table 2
6.2 rate of recovery and precision
Blank sample is chosen, the hybrid standard working solution of 3 concentration levels is accurately added respectively, by 4 pre-treatment side
Method is handled, be measured in parallel 6 parts, detected under conditions of 5.1,5.2, calculate average recovery rate, measured value it is opposite
Standard deviation, in a few days day to day precision.The result shows that the average recovery rate of object reaches in each object rate of recovery
67.4%~119.13%, relative standard deviation (n=6) between 0.66%~10.78%, withinday precision (n=6)≤
9.12%, day to day precision (n=3)≤10.46% the results are shown in Table 3.
Table 3
Embodiment 2
The blood sample of 10 doubtful herbicide poisonings is detected using the method for embodiment 1.
The pre-treating method employed in the 4 of embodiment 1 carries out albumen precipitation to blood sample to be measured, 5.1,5.2
Under conditions of detected, as a result detect 1 paraquat 7 (blood middle concentration be 0.09~78.48 μ g/ml), glyphosate (blood
Concentration is 0.79 μ g/ml in liquid), atrazine 1 (blood middle concentration 4.73ng/ml), (blood middle concentration is Acetochlor 1
10.57ng/ml)。
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (7)
1. the screening of common herbicide, quantitative detecting method in a kind of blood, which is characterized in that with precipitation of protein to blood sample into
Row pre-treatment detects the herbicide in the blood sample with liquid chromatogram/high resolution mass spectrum combination analysis method.
2. the screening of common herbicide, quantitative detecting method in blood according to claim 1, which is characterized in that described
The concrete operation step of precipitation of protein is：The albumen precipitation for being equivalent to 4~5 times of volumes of blood sample is added into the blood sample
Agent, be vortexed 60~90s, after 5~10min of ultrasound, 10000~12000rpm/min, 10~15min of centrifugation, take supernatant to get；
Wherein, the protein precipitant is 70~80v/v% acetonitrile solution.
3. the screening of common herbicide, quantitative detecting method in blood according to claim 1, which is characterized in that described
In liquid chromatogram/high resolution mass spectrum combination analysis method, the chromatographic condition of the liquid chromatogram is：
Chromatographic column：Octadecylsilane chemically bonded silica chromatographic column；
Mobile phase A is 0.1% formic acid solution, and Mobile phase B is methanol, carries out linear gradient elution, the linear eluent gradient is such as
Under：
Flow velocity：0.3mL/min.
4. the screening of common herbicide, quantitative detecting method in blood according to claim 1, which is characterized in that described
In liquid chromatogram/high resolution mass spectrum combination analysis method, the analysis condition of the high resolution mass spectrum is：
Ion source：The source HESI；
Electron spray voltage：3200V；
Capillary temperature：320℃；
Auxiliary heater temperature：300℃；
Sheath gas：Nitrogen, flow velocity 30L/min；
Assist gas：Nitrogen, flow velocity 15L/min；
Data scanning mode：The level-one full scan of positive and negative switching/real-time secondary scanning of the mass spectrum mode, the level-one full scan mode
Resolution ratio be 70000, the resolution ratio of second level scan pattern is 17500.
5. the screening of common herbicide, quantitative detecting method in blood according to claim 1, which is characterized in that described
The type of herbicide includes quaternary ammonium salt, organic phosphates, triazine, imidazolone type, amides, sulfonylurea, diphenyl ether
Class, phenoxy carboxylic acid, benzoic acids, aryloxyphenoxypropionic class, dinitroaniline, picolinic acid class and cyclohexenone analog
At least one of.
6. the screening of common herbicide, quantitative detecting method in blood according to claim 5, which is characterized in that quaternary ammonium
Salt herbicide includes at least one of paraquat and diquat dibromide；And/or
Organic phosphates herbicide includes at least one of glyphosate and glufosinate-ammonium；And/or
Triazine herbicide includes at least one of cyanazine, atrazine, Simanex, symetryne and prometryn；And/or
Imidazolinone herbicide includes at least one of imazapyr；And/or
Acetamide-group herbicides include at least one of metazachlor, Acetochlor and propisochlor；And/or
Sulfonylurea herbicide includes at least one of chlorsulfuron, metsulfuron-methyl, bensulfuron-methyl and oxasulfuron；And/or
Diphenyl ether herbicide is Bentazon；And/or
Benzene oxycarboxylic acid and benzoic acid herbicide are dicamba；And/or
Aryloxyphenoxypropionic class herbicide includes at least one of haloxyfop-P-methyl and quizalofop-ethyl；And/or
Dinitroaniline herbicide includes at least one of Pendimethalin and Amex820；And/or
Picolinic acid class herbicide is clopyralid；And/or
Cyclohexenone analog herbicide is alloxydimsodium.
7. the screening of common herbicide, quantitative detecting method determine Toxicosis Death in legal medical expert in blood described in a kind of claim 1
The application of herbicide type and content in blood sample is analyzed in the process.
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| CN114965840A (en) * | 2021-02-24 | 2022-08-30 | 公安部物证鉴定中心 | Method for detecting glyphosate, glufosinate-ammonium and metabolites in organism liquid |
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| CN108918709B (en) | 2021-05-18 |
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