CN104614478B - A kind of assay method of Pyrifluquinazon residual quantity - Google Patents
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Abstract
The invention discloses a kind of assay method of Pyrifluquinazon residual quantity, the method is mainly used in the method measuring Pyrifluquinazon content residual in the complex matrices such as Cereals, animal derived food food agricultural product.Pyrifluquinazon residual in sample is extracted, C with acetonitrile or containing the acetonitrile solution homogeneous of 1% acetic acid
18after/PSA Solid-Phase Extraction column purification is concentrated, Gas Chromatography-Negative chemical ionization source-mass spectrum (GC-NCI-MS) detects, and adopts and does not set up the typical curve corrected, quantified by external standard method containing the vehicle solution of agricultural chemicals to be measured.This method average recovery rate is 75.1% ~ 80.2%, average relative standard's deviation (RSD) is 4.8% ~ 8.0%, detection limit lower than 2.77 μ g/kg, have easy and simple to handle, quick, impurity elimination is effective, highly sensitive, characteristic is strong, reproducible, qualitative, quantitative advantage accurately.The 0.01mg/kg residue limits of the countries such as Japan, European Union, Korea S to corresponding food safety detection being met, i.e. the technical requirement of " uniform limit ", providing strong technical support by for ensureing that our people's food security and export abroad trade develop in a healthy way.
Description
Technical field
The present invention relates to a kind of assay method of Pyrifluquinazon residual quantity, be more particularly the method adopting Gas Chromatography-Negative chemical ionization source-mass spectrum (GC-NCI-MS) qualitative, quantitative to measure Pyrifluquinazon content residual in the animals and plants derived food of the complex matrices such as animal muscle and goods such as Cereals, pork, beef, mutton, chicken, belong to the determination techniques field of persticide residue.
Background technology
The invention of Japanese agricultural chemicals company of Pyrifluquinazon system, and the new quinazoline ditosylate salt pesticide of the tool biamide structure developed jointly in Japanese combinatorial chemistry company, to be mainly used on control vegetables, fruit tree and tealeaves the sucking insects such as Phytophthira, aleyrodid class, mealybug class, leafhopper class, thrips class.Chemistry 1-acetyl group-3,4-dihydro-3-by name [(3-pyridylmethyl) is amino]-6-[1,2; 2; the fluoro-1-of 2-tetra-(trifluoromethyl) ethyl]-2-(1H)-quinazolinone, CAS accession number is 337458-27-2, and structural formula is:
Pyrifluquinazon is used for 18 kinds of crops such as vegetables, tea tree and fruit tree on October 20th, 2010 in Japan's registration, and insect is planted in control more than 20.The former medicine pyrifluquinazon of new pesticides that in January, 2013, Environmental Protection in America was deployed on suggestion approval NichinoAmerica company registers and sucks insect as aphid for greenhouse ornamental crops prevention and control, thrips, aleyrodid etc.This pharmacy effect mechanism makes insect stop taking food and then dying of hunger, and can prevent plant tissue from suffering more infringement, with the propagation of some important diseases of limit.In view of this medicament has novel mechanism of action, the insect that known insecticides susceptibility is declined can be prevented and treated well, and fool proof to various natural enemy, be therefore very suitable for pest resistance management and the comprehensive regulation, there is good application prospect and very large application market.
Although Pyrifluquinazon is little to neurotoxicity and Genotoxic Effect, to the toxic effect of testis, liver and blood pressure.Therefore, the Korea S as agricultural product main exit markets such as China's veterinary antibiotics has formulated residue limits standard with Japan to it.The maximum maximum permission quantity of Korea S regulation Pyrifluquinazon on apple and pears is 0.05mg/kg; Japan has formulated pyrifluquinazon and metabolin B (1,2,3,4-tetrahydrochysene-3-[(3-picolyl) amine]-6-[1, the fluoro-1-of 2,2,2-tetra-(trifluoromethyl) ethyl] quinazoline-2-one) be scaled pyrifluquinazon's and residue limits standard, the residue limits be defined on apple, pears, potato is respectively 0.5,1,0.2mg/kg, all the other are all carried out " uniform limit " of 0.01mg/L; European Union carries out " uniform limit " of 0.01mg/L to pyrifluquinazon.
Up to now, there is 1 section abroad about the report of Pyrifluquinazon residues detection method in food, this detection method adopts acetonitrile to extract, liquid liquid distributes and after the purification of silica gel solid-phase extraction column, liquid chromatography-UV-detector (HPLC-UVD) detects Pyrifluquinazon residual quantity; Domesticly only retrieve a patent " a kind of assay method of Pyrifluquinazon residual quantity ", this patent establishes the detection method adopting Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) to measure Pyrifluquinazon residual quantity in vegetables and fruit.Because food substrate is more complicated, preferably adopt when residues of pesticides are analyzed and can carry out accurately detection method qualitatively, as gaschromatographic mass spectrometry, gas chromatography tandem mass spectrum or liquid chromatography tandem mass spectrometry.Use LC-MS/MS to measure food Residual Pesticides in Farm Produce and there is quick, easy, sensitivity advantages of higher, but due to its price costly, a lot of testing agency, enterprise or scientific research institutions do not configure this instrument or configuration number of units is less, during due to different compounds employing LC-MS/MS detection, different mobile phases or chromatographic column need be used, such needs constantly change chromatographic column, mobile phase expend the long time and balance system, and this constrains the application of LC-MS/MS to a certain extent.The gaschromatographic mass spectrometry (GC-NCI-MS) in outfit negative chemical ionization source is analyzed food Residual Pesticides in Farm Produce tool and is had great advantage, Negative chemical ionization (NCI source) is called as mass spectrum " soft ionization source ", to the analysis thing containing electronegativity group, there is high selectivity and high sensitivity, because its characteristic is strong, when utilizing it to carry out retention analysis, matrix interference is little, can carry out qualitative and quantitative analysis very accurately to object.Existing various testing agency and enterprise have all purchased gas chromatograph-mass spectrometer (GCMS) (GC-MS), generally also be provided with Negative chemical ionization (NCI), now a lot of class agricultural chemicals is all containing electronegativity group, and organochlorine and pyrethroid pesticide molecule are mostly containing strong electronegative group such as-F ,-Cl ,-Br or-COO-, organophosphorus pesticide molecule is mostly containing the=electronegativity group such as S ,-OR ,-P ,-O-,-Cl or-P=O, and mostly containing-F group in the novel agrochemical developed in recent years, therefore, use GC-NCI-MS conveniently can realize the multi-residue analysis of Multiple Pesticides, compared with GC-NCI-MS, better antijamming capability can be obtained, lower sensitivity and better selectivity, Pyrifluquinazon belongs to electronegativity compound, but have no the report of the GC-NCI-MS detection method of Pyrifluquinazon residual quantity in vegetables and fruit up to now, due to Cereals, the food agricultural product matrix more complicated such as animal derived food, the good sample-pretreating method of clean-up effect must be set up and instrumental conditions could meet testing requirement, therefore, the detection method setting up Pyrifluquinazon residual quantity in Gas Chromatography-Negative chemical ionization source-mass spectrum (GC-NCI-MS) qualitative and quantitative analysis Cereals and animal derived food is significant.
Summary of the invention
The object of this invention is to provide a kind of assay method of Pyrifluquinazon residual quantity, be mainly used in measuring Pyrifluquinazon residual quantity in the complex matrices such as Cereals, animal derived food food agricultural product.
For realizing above object, the technical solution adopted in the present invention is: a kind of assay method of Pyrifluquinazon residual quantity, comprises the steps:
(1) extract
Take mixing sample in tool plug centrifuge tube, after adding suitable quantity of water recovery, quantitatively add acetonitrile or extract containing the acetonitrile solution homogeneous of 1% acetic acid or oscillating ultrasonic, then adding the one in sodium chloride or sodium acetate and anhydrous magnesium sulfate, centrifugal after violent vortex 1min.
(2) purify
Pipette certain volume sample extracting solution, be concentrated into about 1mL, through C
18/ PSA Solid-Phase Extraction column purification, acetonitrile, collects eluent, is concentrated into after doing, and dissolves constant volume, after crossing film, treat that Gas Chromatography-Negative chemical ionization source-mass spectrum (GC-NCI-MS) detects with acetone/normal hexane mixed solvent that volume ratio is 1/1.
(3) preparation of standard working solution
When same kind matrix blank sample not containing Pyrifluquinazon is processed by above-mentioned steps (1), (2), obtain sample extraction purification residue, add appropriate solvent and mixed standard solution, vortex mixes, and is mixed with the Pyrifluquinazon series hybrid standard working fluid of at least 3 concentration.
(4) Gas Chromatography-Negative chemical ionization source-mass spectroscopy (GC-NCI-MS) measures
The standard working solution of each concentration gradient in step (3) is carried out GC-NCI-MS mensuration, with the chromatographic peak area of standard working solution, regretional analysis is carried out to its respective concentration, obtain standard working curve; Under the same conditions the sample liquid after purification in step (2) is injected GC-NCI-MS to measure, record the chromatographic peak area of Pyrifluquinazon in sample liquid, substitute into typical curve, obtain Pyrifluquinazon content in sample liquid, then representated by liquid, the Mass Calculation of sample obtains Pyrifluquinazon residual quantity in sample per sample.
Step (1), if the sample of the middle moisture content less such as sample Cereals and animal's liver, must add suitable quantity of water and fully infiltrate before extraction.
Add sodium chloride when adopting acetonitrile to extract in step (1) to saltout, add sodium acetate when adopting the acetonitrile solution containing 1% acetic acid to extract and saltout.
Step carries out C in (2)
18/ PSA Solid phase extraction, during acetonitrile, elution volume is 6 ~ 8mL.
In step (4), GC conditions is: chromatographic column: HP-5MS capillary chromatographic column, column length 30m, internal diameter 0.25mm, thickness 0.25 μm; Injector temperature 250 DEG C; Carrier gas: He, not shunt mode sample introduction, sample size: 1 μ L; Constant current mode, flow velocity 1.0mL/min; Heating schedule: initial temperature 60 DEG C keeps 2min, rises to 200 DEG C, then rises to 220 DEG C with the speed of 2 DEG C per minute, then rise to 280 DEG C with the speed of 20 DEG C per minute with the speed of 20 DEG C per minute, keeps 10min; Transmission line temperature: 280 DEG C.
In step (4), Mass Spectrometry Conditions is: ion source temperature 150 DEG C; Quadrupole rod temperature 150 DEG C; Ionization pattern: negative chemical ionization, i.e. NCI pattern, energy 70eV; Scan mode: Salbutamol Selected Ion Monitoring (SIM) pattern; The solvent delay time is 10min; The ion of monitoring is: 444,337,402,309.
When measuring sample liquid and extraction standard working solution in step (4), if sample liquid Pesticides chromatographic peak retention time agricultural chemicals retention time corresponding to standard solution is consistent, and in the sample mass spectrogram after background correction, selected ion all occurs, and abundance of ions than with the abundance of ions of standard solution than consistent, then can judge to exist in sample liquid this agricultural chemicals; If above-mentioned two conditions can not meet simultaneously, then judge not containing this kind of agricultural chemicals.
Beneficial effect of the present invention is:
The present invention utilizes dispersive solid-phase extraction technology, establish sample-pretreating method that is easy, that also can effectively avoid sample mesostroma to disturb fast, this pre-treating method to be applied in Cereals, animal derived food the qualitative confirmation of Pyrifluquinazon in conjunction with GC-NCI-MS and quantitatively to detect, average recovery rate is 75.1% ~ 80.2%, average relative standard's deviation (RSD) is 4.8% ~ 8.0%, detection limit, lower than 2.77 μ g/kg, has easy and simple to handle, quick, accurate, highly sensitive and reproducible advantage.The 0.01mg/kg residue limits of the countries such as Japan, European Union, Korea S to corresponding food safety detection being met, i.e. the technical requirement of " uniform limit ", providing strong technical support by for ensureing that our people's food security and export abroad trade develop in a healthy way.
Accompanying drawing explanation
Fig. 1 is the Selective ion mode chromatogram that the 100ng/mLPyrifluquinazon be added in blank pork matrix marks liquid.
Fig. 2 is not containing the Selective ion mode chromatogram of the pork blank sample of Pyrifluquinazon.
The Pyrifluquinazon standard working curve that Fig. 3 is is substrate preparation with the pork blank sample not containing Pyrifluquinazon.
Embodiment
Now with following embodiment, the present invention is described, but is not limit the scope of the invention.
The instrument used in embodiment and reagent
T18Basic homogenizer (IKA, Germany); CR21G III hydro-extractor (Hitachi, Japan); MS3 basic model vortex mixer (IKA, Germany); TurboVapLV type sample automatic concentration instrument (Caliper, USA); 7890N gas chromatography-5975C mass spectrometer (Agilent, USA); C
18/ PSA solid-phase extraction column (6mL, 500mg/500mg) is purchased from Tianjin Bonaaijieer Technology Co., Ltd.
Reagent: acetonitrile, acetone, normal hexane (HPLC level, Merke, Germany); Acetic acid (HPLC level, CNW, Germany); Anhydrous magnesium sulfate, sodium chloride and sodium acetate are pure for analyzing, all purchased from Chemical Reagent Co., Ltd., Sinopharm Group.
Standard substance: 100mg/L, acetontrile, purchased from German Dr.Ehrenstorfer company.
Embodiment 1: the detection of Pyrifluquinazon residual quantity in pork
(1) sample pre-treatments
Extract
Take 5g pork sample through fully mixing in 50mL centrifuge tube, add the mixing of 5mL water, place 30min, accurately add 20mL acetonitrile, homogeneous extracts 2min, adds 3g anhydrous magnesium sulfate and 2g sodium chloride, after vortex 1min, and the centrifugal 5min of 7000r/min.After centrifugal, get 8mL acetonitrile extract in 40 DEG C revolve steaming or nitrogen blow to about 1mL, to be clean.
Purification
With 5mL acetonitrile prewashing C
18/ PSA solid-phase extraction column, when liquid level arrives the top of adsorbent, said extracted solution is proceeded in post, with 2mL acetonitrile wash test tube, and cleansing solution is moved in SPE post, when solution reaches adsorbent top, add on 4mL acetonitrile to pillar and carry out wash-out, eluent all receives in quantitative test tube, nitrogen dry up rear volume ratio be 1/1 acetone/normal hexane mixed solvent be settled to 1mL, after crossing 0.22 μm of filter membrane, treat that GC-NCI-MS measures.
(2) preparation of standard working solution
By 100ng/mL standard solution volume ratio be 1/1 acetone/normal hexane mixed solvent be diluted to 10ng/mL standard intermediate liquid, by 10 μ g/mL standard solution dilution be made into 5,2,1,0.5,0.2,0.1 μ g/mL standard solution.Pork blank sample not containing Pyrifluquinazon is pressed above-mentioned pre-treatment step process, obtain sample extraction purification residue, acetone/normal hexane mixed solvent and the above-mentioned mixed standard solution of 100 μ L that 900 μ L volume ratios are 1/1 is added in this residue, vortex mixes, and is made into 10,20,50,100,200,500 μ g/L extraction standard working solutions.
(3) Gas Chromatography-Negative chemical ionization source-mass spectroscopy (GC-NCI-MS) measures
The standard working solution of variable concentrations gradient is injected GC-NCI-MS respectively, carries out the quantitative test of Pyrifluquinazon content with external standard method, namely with the chromatographic peak area of standard working solution, regretional analysis is carried out to its respective concentration, obtain typical curve; Under the same conditions sample extracting solution is injected GC-NCI-MS to measure, record the chromatographic peak area of Pyrifluquinazon in sample liquid, substitute into typical curve, obtain Pyrifluquinazon content in sample liquid, then representated by liquid, the Mass Calculation of sample obtains Pyrifluquinazon residual quantity in sample per sample.
Wherein chromatographic condition is:
Chromatographic column: HP-5MS capillary chromatographic column, column length 30m, internal diameter 0.25mm, thickness 0.25 μm.
Injector temperature: 250.0 DEG C, sample introduction pattern: Splitless injecting samples, sample size: 1 μ L.
Carrier gas: He, constant current mode, flow velocity 1.0mL/min.
Stove case heating schedule: initial temperature 60 DEG C keeps 2min, rises to 200 DEG C, then rises to 220 DEG C with the speed of 2 DEG C per minute, then rise to 280 DEG C with the speed of 20 DEG C per minute with the speed of 20 DEG C per minute, keeps 10min.
Transmission line temperature: 280 DEG C.
Wherein, mass spectrometry parameters is:
Ionization pattern: negative chemical ionization, i.e. NCI pattern, energy 70eV.
Ion source temperature: 150 DEG C; Quadrupole rod temperature 150 DEG C.
Scan mode: Salbutamol Selected Ion Monitoring (SIM) pattern; The solvent delay time is 10min; The ion of SIM monitoring is: 444,337,402,309; Quota ion is 444.
Qualitative Identification: at identical conditions, if sample liquid Pesticides chromatographic peak retention time agricultural chemicals retention time corresponding to standard solution is consistent, and in the sample mass spectrogram after background correction, selected ion all occurs, and abundance of ions than with the abundance of ions of standard solution than consistent, then can judge to exist in sample liquid this agricultural chemicals; If above-mentioned two conditions can not meet simultaneously, then judge not containing this kind of agricultural chemicals.
With the chromatographic peak area of standard working solution, regretional analysis is carried out to its respective concentration, obtain standard working curve as table 1.
The typical curve of Pyrifluquinazon in table 1 pork bare substrate
| Title | Retention time (min) | Regression equation | Related coefficient |
| Pyrifluquinazon | 22.52 | Y＝39.192X-322.8 | 0.9997 |
Recovery of standard addition and repeatability:
In the pork not containing Pyrifluquinazon, add the Pyrifluquinazon standard solution of 10, a 20 and 200 μ g/kg3 concentration level, add after 30min until agricultural chemicals and carry out the determination of residual amount by above-mentioned treatment step.Mensuration concentration and agricultural chemicals theory are added concentration compare, obtain agricultural chemicals TIANZHU XINGNAO Capsul, each Pitch-based sphere replicate determination 6 times, obtain its relative standard deviation, measurement result is in table 2.As can be seen from Table 2, in 3 mark-on levels, the average recovery rate of Pyrifluquinazon is 75.1% ~ 79.7%, and average relative standard's deviation (RSD) is 5.5% ~ 7.7%, illustrates that the recovery of the inventive method is higher, reproducible.
The recovery of table 2Pyrifluquinazon and repeatability (n=6)
Detection limit:
The Pyrifluquinazon extraction standard working solution of variable concentrations is injected GC-NCI-MS, calculate detection limit with the cycles of concentration (cycles of concentration of pork is 2.0 times) of 3 times of signal to noise ratio (S/N ratio)s of least concentration extraction standard solution chromatographic peak and sample handling processes, detecting of Pyrifluquinazon is limited to 2.77 μ g/kg.
Embodiment 2: the detection of Pyrifluquinazon residual quantity in wheat
(1) sample pre-treatments
Extract
Take 5g wheat samples (grinding to form flour) through fully mixing in 50mL centrifuge tube, after adding 20mL water recovery 30min, accurately add the acetonitrile solution of 20mL containing 1% acetic acid, mechanical shaking extraction 20min, ultrasonic extraction 5min, add 3g anhydrous magnesium sulfate and 2g sodium acetate, after vortex 1min, the centrifugal 5min of 7000r/min.After centrifugal, get 8mL acetonitrile extract and revolve steaming or nitrogen blows near dry in 40 DEG C, after adding 1mL acetonitrile vortex, to be clean.
Purification
With 5mL acetonitrile prewashing C
18/ PSA solid-phase extraction column, when liquid level arrives the top of adsorbent, said extracted solution is proceeded in post, with 2mL acetonitrile wash test tube, and cleansing solution is moved in SPE post, when solution reaches adsorbent top, add on 4mL acetonitrile to pillar and carry out wash-out, eluent all receives in quantitative test tube, nitrogen dry up rear volume ratio be 1/1 acetone/normal hexane mixed solvent be settled to 1mL, after crossing 0.22 μm of filter membrane, treat that GC-NCI-MS measures.
(2) preparation of standard working solution
By 100ng/mL standard solution volume ratio be 1/1 acetone/normal hexane mixed solvent be diluted to 10ng/mL standard intermediate liquid, by 10 μ g/mL standard solution dilution be made into 5,2,1,0.5,0.2,0.1 μ g/mL standard solution.Wheat blank sample not containing Pyrifluquinazon is pressed above-mentioned pre-treatment step process, obtain sample extraction purification residue, acetone/normal hexane mixed solvent and the above-mentioned mixed standard solution of 100 μ L that 900 μ L volume ratios are 1/1 is added in this residue, vortex mixes, and is made into 10,20,50,100,200,500 μ g/L extraction standard working solutions.
(3) Gas Chromatography-Negative chemical ionization source-mass spectroscopy (GC-NCI-MS) measurement operation step, chromatogram and Mass Spectrometry Conditions are consistent with the mensuration of Pyrifluquinazon in above-mentioned pork sample.
Qualitative Identification: consistent with the mensuration of Pyrifluquinazon in above-mentioned pork sample.
Linear relationship:
Carry out regretional analysis with the chromatographic peak area of standard working solution to its respective concentration, obtaining standard working curve is Y=44.35X-312.73, and related coefficient is 0.9996.
Recovery of standard addition and repeatability:
The Pyrifluquinazon standard solution of 10, a 20 and 200 μ g/kg3 concentration level is added in the wheat not containing Pyrifluquinazon, add after 30min until agricultural chemicals and carry out the determination of residual amount by above-mentioned treatment step, mensuration concentration and agricultural chemicals theory are added concentration compare, obtain agricultural chemicals TIANZHU XINGNAO Capsul, each Pitch-based sphere replicate determination 6 times, obtain its relative standard deviation, measurement result is in table 3.As can be seen from Table 3, in 3 mark-on levels, the average recovery rate of Pyrifluquinazon is 78.3% ~ 80.2%, and average relative standard's deviation (RSD) is 4.8% ~ 8.0%, illustrates that the recovery of the inventive method is high, reproducible.
The recovery of table 3Pyrifluquinazon and repeatability (n=6)
Detection limit:
The Pyrifluquinazon extraction standard working solution of variable concentrations is injected GC-NCI-MS, calculate detection limit with the cycles of concentration (cycles of concentration of wheat is 2.0 times) of 3 times of signal to noise ratio (S/N ratio)s of least concentration extraction standard solution chromatographic peak and sample handling processes, detecting of Pyrifluquinazon is limited to 2.42 μ g/kg.
Above embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various modification that the common engineering in this area is made technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.
Claims (4)
1. an assay method for Pyrifluquinazon residual quantity, is characterized in that, said method comprising the steps of:
(1) extract
Take mixing sample in tool plug centrifuge tube, after adding suitable quantity of water, add acetonitrile or after extracting containing the acetonitrile solution homogeneous of 1% acetic acid or oscillating ultrasonic, add the one in sodium chloride or sodium acetate and anhydrous magnesium sulfate, centrifugal after violent vortex 1min;
(2) purify
Pipette certain volume sample extracting solution, be concentrated into about 1mL, through C
18/ PSA Solid-Phase Extraction column purification, acetonitrile, collects eluent, is concentrated into after doing, and dissolves constant volume, after crossing film, treat that Gas Chromatography-Negative chemical ionization source-mass spectrum (GC-NCI-MS) detects with acetone/normal hexane mixed solvent that volume ratio is 1/1;
(3) preparation of standard working solution
Same kind matrix blank sample not containing Pyrifluquinazon is processed by above-mentioned steps (1), (2), obtain sample extraction purification residue, add appropriate solvent and standard solution, vortex mixes, and is mixed with the Pyrifluquinazon series standard working fluid of at least 3 concentration;
(4) mensuration and result calculate
GC-NCI-MS analysis condition is: chromatographic column: HP-5MS capillary chromatographic column, column length 30m, internal diameter 0.25mm, thickness 0.25 μm; Injector temperature 250.0 DEG C; Carrier gas: He, not shunt mode sample introduction, sample size: 1 μ L; Constant current mode, flow velocity 1.0mL/min; Heating schedule: initial temperature 60 DEG C keeps 2min, rises to 200 DEG C, then rises to 220 DEG C with the speed of 2 DEG C per minute, then rise to 280 DEG C with the speed of 20 DEG C per minute with the speed of 20 DEG C per minute, keeps 10min; Transmission line temperature: 280 DEG C; Ionization pattern: negative chemical ionization, i.e. NCI pattern, energy 70eV; Ion source temperature 150 DEG C; Scan mode: Salbutamol Selected Ion Monitoring (SIM) pattern, the ion of monitoring is: 444,337,402,309;
The standard working solution of each concentration gradient in step (3) is carried out GC-NCI-MS mensuration, with the chromatographic peak area of standard working solution, regretional analysis is carried out to its respective concentration, obtain extraction standard working curve; Under the same conditions the sample liquid after purification in step (2) is injected GC-NCI-MS to measure, record the chromatographic peak area of Pyrifluquinazon in sample liquid, substitute into extraction standard curve, obtain Pyrifluquinazon content in sample liquid, then representated by liquid, the Mass Calculation of sample obtains Pyrifluquinazon residual quantity in sample per sample.
2. the assay method of a kind of Pyrifluquinazon residual quantity according to claim 1, is characterized in that, step (1), if middle sample Cereals and animal's liver sample, must add suitable quantity of water and fully infiltrate before extraction.
3. the assay method of a kind of Pyrifluquinazon residual quantity according to claim 1, it is characterized in that, sodium chloride need be added when adopting acetonitrile to extract in step (1) to saltout, sodium acetate need be added when adopting the acetonitrile solution containing 1% acetic acid to extract and saltout.
4. the assay method of a kind of Pyrifluquinazon residual quantity according to claim 1, is characterized in that, step carries out C in (2)
18/ PSA Solid phase extraction, during acetonitrile, elution volume is 6 ~ 8mL.
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| Title |
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| Application of Multi-residue Analytical Method to 6 Agricultural Products;Shigeki AKAMATSU 等;《兵庫県立健康生活科学研究所健康科学研究センタ一研究报告 第5号》;20140627;第1-12页 * |
| Development and validation of analytical methods for pyrifluquinazon residues determination on agricultural commodities by HPLC-UVD;Jung-Ah Do 等;《Analytical Science & Technology》;20130630;第26卷(第3期);第174-181页 * |
| 夏广辉 等.气相色谱⁃ * |
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