CN106018571A - Detection method for residual amount of chlorantraniliprole in aquatic vegetables - Google Patents
Detection method for residual amount of chlorantraniliprole in aquatic vegetables Download PDFInfo
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- CN106018571A CN106018571A CN201510750915.9A CN201510750915A CN106018571A CN 106018571 A CN106018571 A CN 106018571A CN 201510750915 A CN201510750915 A CN 201510750915A CN 106018571 A CN106018571 A CN 106018571A
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- Prior art keywords
- acetone
- ethyl acetate
- methanol
- standard
- rynaxypyr
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- PSOVNZZNOMJUBI-UHFFFAOYSA-N chlorantraniliprole Chemical compound CNC(=O)C1=CC(Cl)=CC(C)=C1NC(=O)C1=CC(Br)=NN1C1=NC=CC=C1Cl PSOVNZZNOMJUBI-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 235000013311 vegetables Nutrition 0.000 title claims abstract description 16
- 238000001514 detection method Methods 0.000 title abstract description 15
- 239000005886 Chlorantraniliprole Substances 0.000 title abstract 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 45
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000012086 standard solution Substances 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 48
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 6
- 230000008014 freezing Effects 0.000 claims description 6
- 238000007710 freezing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000002203 pretreatment Methods 0.000 claims description 6
- 239000011550 stock solution Substances 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000002390 rotary evaporation Methods 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000460 chlorine Substances 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- 239000012224 working solution Substances 0.000 claims description 4
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical class NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 abstract description 5
- 239000003463 adsorbent Substances 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 3
- 238000002414 normal-phase solid-phase extraction Methods 0.000 abstract description 3
- 239000000945 filler Substances 0.000 abstract description 2
- 230000002452 interceptive effect Effects 0.000 abstract description 2
- 239000000049 pigment Substances 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract 2
- CFNHVUGPXZUTRR-UHFFFAOYSA-N n'-propylethane-1,2-diamine Chemical compound CCCNCCN CFNHVUGPXZUTRR-UHFFFAOYSA-N 0.000 abstract 1
- 150000007524 organic acids Chemical class 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 abstract 1
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 12
- 239000007789 gas Substances 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 238000004949 mass spectrometry Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 240000000260 Typha latifolia Species 0.000 description 3
- 235000005324 Typha latifolia Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 238000002552 multiple reaction monitoring Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- 241000255777 Lepidoptera Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 241000607479 Yersinia pestis Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 239000002917 insecticide Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 241000590412 Agromyzidae Species 0.000 description 1
- 241000254127 Bemisia tabaci Species 0.000 description 1
- KXDAEFPNCMNJSK-UHFFFAOYSA-N Benzamide Chemical compound NC(=O)C1=CC=CC=C1 KXDAEFPNCMNJSK-UHFFFAOYSA-N 0.000 description 1
- 241001347514 Carposinidae Species 0.000 description 1
- 241001124134 Chrysomelidae Species 0.000 description 1
- 241000254173 Coleoptera Species 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 206010033799 Paralysis Diseases 0.000 description 1
- 241000500437 Plutella xylostella Species 0.000 description 1
- 241000255893 Pyralidae Species 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 210000000805 cytoplasm Anatomy 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 1
- -1 machine is sour Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 102000042094 ryanodine receptor (TC 1.A.3.1) family Human genes 0.000 description 1
- 108091052345 ryanodine receptor (TC 1.A.3.1) family Proteins 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a detection method characterized by good stability and high sensitivity for the residual amount of chlorantraniliprole in aquatic vegetables. The method comprises the steps of: (1) preparation of a standard solution; (2) preparation of a solvent; (3) a pretreatment extraction process; and (4) determination: taking the filtrate obtained in step (1) and step (3) to conduct liquid chromatography-tandem mass spectrometry determination. The detection method for the residual amount of chlorantraniliprole in aquatic vegetables uses a mixed solvent of ethyl acetate and acetone (V/V 7:3) to extract chlorantraniliprole residue in aquatic vegetables, purification by a dispersive solid-phase extraction N-propyl ethylenediamine (PSA) adsorbent is conducted, and then the characteristics of strong selectivity and anti-interference capability of liquid chromatography-tandem mass spectrometry are utilized to determine the residual amount. By using the ethyl acetate:acetone (V/V 7:3) mixed solvent, the extraction efficiency is high, and little extraction matrix interference exists. By using the PSA filler as the adsorbent, the extracted organic acid, pigments and other interfering substances can be removed so as to achieve the purpose of purification.
Description
Technical field
The present invention relates to the detection method of a kind of aquatic vegetable residual, chlorine in especially a kind of detection aquatic vegetable
The method of worm Benzoylamide residual quantity.
Background technology
Rynaxypyr is the new and effective broad spectrum pesticide of one of E.I.Du Pont Company's exploitation, to lepidopterous night
Moth section, Pyralidae, Carposinidae, tortricid, miller section, diamond-back moth section, Gelechidae, Gracilariidae etc. are equal
Have and well control effect, moreover it is possible to control coleoptera Culculionidae, Chrysomelidae;Diptera Agromyzidae;Bemisia tabaci
Etc. multiple non-lepidoptera pest.Rynaxypyr can efficiently activate insecticide ryanodine receptor, destroys Cytoplasm
Interior Ca2+Ambient stable, causes insecticide paralysis death, high to the larva activity of lepidoptera pest, has fast
Speed stops insect feed, to be efficiently detained activity, resistance of rainwater washing against, permeability strong.
Report relatively about the method for Rynaxypyr residues detection in veterinary antibiotics the most both at home and abroad
Many, main employing high performance liquid chromatography and LC/MS, its pre-treatment Extraction solvent is predominantly
Acetonitrile or acid acetonitrile, and not yet have about the method for Rynaxypyr residues detection in aquatic vegetable
Report.
Summary of the invention
The invention provides Rynaxypyr in a kind of good stability, highly sensitive detection aquatic vegetable residual
The method of allowance.
Realize the method for Rynaxypyr residual quantity in the detection aquatic vegetable of the object of the invention, including as follows
Step:
(1) preparation of standard solution:
Accurately weigh 10mg chlorine worm this Methanamide standard substance in 10mL volumetric flask, dissolve constant volume with methanol
To scale, being configured to concentration is 1mg/mL Standard Stock solutions, is placed in-18 DEG C of refrigerators freezing lucifuge and protects
Deposit;
Accurately a certain amount of 1mg/mL Rynaxypyr Standard Stock solutions of absorption is in volumetric flask, uses first
It is 10 μ g/mL intermediate concentration standard solution that alcohol is diluted to mass concentration, is placed in 4 DEG C of refrigerators freezing lucifuge and protects
Deposit;
Accurately draw a certain amount of 10 μ g/mL Rynaxypyr intermediate concentration standard solution, use first respectively
Alcohol and water mixed solution (V/V 3: 7) stepwise dilution are 2ng/mL, 5ng/mL, 10ng/mL to concentration,
The standard working solution of 20ng/mL, 50ng/mL and 100ng/mL, matching while using;
(2) preparation of solvent:
Ethyl acetate: acetone (V/V 7: 3) solvent: measure 700mL ethyl acetate and 300mL acetone,
Mix homogeneously;
Methanol and water mixed solution (V/V 3: 7): measure 300mL methanol and 700mL water, mix homogeneously;
(3) pre-treatment extraction process:
Weigh 10.00g sample (being accurate to 0.05g) to be placed in tool plug plastic centrifuge tube, addition ethyl acetate:
Acetone (v/v 7: 3) 20mL, ultrasonic 10min, add the mixing of 3g sodium chloride, and 4000r/min is centrifuged 10min,
Taking the supernatant and add 0.1g PSA powder vortex, it is clear that standing takes 2mL upper strata after PSA powder precipitation
Liquid, is blown to do in 45 DEG C of water-bath rotary evaporations or nitrogen, accurately adds 1.00mL methanol and water mixed solution
After (V/V 3: 7) dissolves, in organic filter membrane of mistake 0.22 μm to sample injection bottle, for Instrumental Analysis;
(4) measure: take step (1) and filtrate that step (3) obtains carries out liquid chromatography-tandem mass spectrometry
Instrument measures.
The having the beneficial effect that of method of Rynaxypyr residual quantity in the detection aquatic vegetable of the present invention:
The method of Rynaxypyr residual quantity, use ethyl acetate: third in the detection aquatic vegetable of the present invention
Ketone (V/V 7: 3) mixed solvent extracts Rynaxypyr residual in aquatic vegetable, is dispersed through type Solid-Phase Extraction
After N-propyl group ethylenediamine (PSA) adsorbent purifies, utilize the strong selectivity of liquid chromatography-tandem mass spectrometry and resist dry
Disturb the characteristic of ability, measure its residual quantity.Use ethyl acetate: acetone (V/V 7: 3) mixed solvent extracts
Efficiency is high, and the matrix interference of extraction is few;Use PSA filler as adsorbent, having of extraction can be removed
The interfering materials such as machine is sour, pigment, reach to purify purpose.Present invention application linear optimizing control substitutes solid phase
Extraction, it is possible to reduce time for sample pretreatment, reduces the consumption of organic solvent, cost-effective, reduces environment
Pollute;The inventive method good stability, highly sensitive, measure for Rynaxypyr residual in aquatic vegetable
Surely the most quickly analysis means is provided.
Accompanying drawing explanation
Fig. 1 is the chromatogram adding 5.0 μ g/kg in blank Rhizoma Nelumbinis.
Fig. 2 is the chromatogram adding 5.0 μ g/kg in blank Typha latifolia L..
Detailed description of the invention
In the detection aquatic vegetable of the present invention, the method for Rynaxypyr residual quantity, comprises the steps:
(1) preparation of standard solution:
Accurately weigh 10mg chlorine worm this Methanamide standard substance in 10mL volumetric flask, dissolve constant volume with methanol
To scale, being configured to concentration is 1mg/mL Standard Stock solutions, is placed in-18 DEG C of refrigerators freezing lucifuge and protects
Deposit;
Accurately a certain amount of 1mg/mL Rynaxypyr Standard Stock solutions of absorption is in volumetric flask, uses first
It is 10 μ g/mL intermediate concentration standard solution that alcohol is diluted to mass concentration, is placed in 4 DEG C of refrigerators freezing lucifuge and protects
Deposit;
Accurately draw a certain amount of 10 μ g/mL Rynaxypyr intermediate concentration standard solution, use first respectively
Alcohol and water mixed solution (V/V 3: 7) stepwise dilution are 2ng/mL, 5ng/mL, 10ng/mL to concentration,
The standard working solution of 20ng/mL, 50ng/mL and 100ng/mL, matching while using;
(2) preparation of solvent:
Ethyl acetate: acetone (V/V 7: 3) solvent: measure 700mL ethyl acetate and 300mL acetone,
Mix homogeneously;
Methanol and water mixed solution (V/V 3: 7): measure 300mL methanol and 700mL water, mix homogeneously;
(3) pre-treatment extraction process:
Weigh 10.00g sample (being accurate to 0.05g) to be placed in tool plug plastic centrifuge tube, addition ethyl acetate:
Acetone (v/v 7: 3) 20mL, ultrasonic 10min, add the mixing of 3g sodium chloride, and 4000r/min is centrifuged 10min,
Taking the supernatant and add 0.1g PSA powder vortex, it is clear that standing takes 2mL upper strata after PSA powder precipitation
Liquid, is blown to do in 45 DEG C of water-bath rotary evaporations or nitrogen, accurately adds 1.00mL methanol and water mixed solution
After (V/V 3: 7) dissolves, in organic filter membrane of mistake 0.22 μm to sample injection bottle, for Instrumental Analysis;
(4) measure: take step (1) and filtrate that step (3) obtains carries out liquid chromatography-tandem mass spectrometry
Instrument measures.
Compound concentration is 2ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 50ng/mL and 100ng/mL
Standard working solution, be analyzed under the following instrument parameter optimized:
Liquid phase chromatogram condition
Chromatographic column: Agilent ZORBAX SB-C18 post 150mm × 2.1mm (i.d.);
Flowing phase: A 0.1% aqueous formic acid, B methanol;
The gradient elution program optimized;
Flow velocity: 0.25mL/min;
Sample size: 25 μ L;
Column temperature: 30 DEG C;
Mass Spectrometry Conditions
Ion source: ESI source
Scan mode: cation scans
Monitoring mode: multiple-reaction monitoring
The mass spectrometry parameters optimized under multiple-reaction monitoring pattern
* quota ion is represented
Ion transfer tube temperature: 350 DEG C
Sheath gas (high pure nitrogen) 40Arb
Auxiliary gas (high pure nitrogen) 10Arb
Collision gas (high-purity argon gas) 1.5m Torr
Spray voltage: 3Kv.
The present invention is according to using ethyl acetate on the basis of the physicochemical property of Rynaxypyr and consulting literatures:
Acetone (v/v 7: 3) mixed solvent is as Extraction solvent, by experimental verification ethyl acetate: acetone (v/v 7: 3) mixes
Bonding solvent is higher than acetonitrile and acid acetonitrile, the matrix interference simultaneously extracted to the extraction efficiency of Rynaxypyr
The most less.The advantage of the method be easy and simple to handle, time-consumingly the shortest, highly sensitive, detection limit is low.
Embodiment 1: the detection of Rynaxypyr residual quantity in Rhizoma Nelumbinis
Sample pre-treatments
Weigh 10.00g Rhizoma Nelumbinis sample (being accurate to 0.05g) to be placed in tool plug plastic centrifuge tube, add acetic acid second
Ester: acetone (v/v 7: 3) 20mL, ultrasonic 10min, adds the mixing of 3g sodium chloride, and 4000r/min is centrifuged
10min, takes the supernatant and adds 0.1g PSA powder vortex, stand and take 2mL after PSA powder precipitation
The supernatant, is blown to do in 45 DEG C of water-bath rotary evaporations or nitrogen, accurately adds 1.00mL methanol: water mixes
After solution (V/V 3: 7) dissolves, in organic filter membrane of mistake 0.22 μm to sample injection bottle, for Instrumental Analysis.
Chromatogram is as shown in Figure 1.
Liquid phase chromatogram condition
Chromatographic column: Agilent ZORBAX SB-C18 post 150mm × 2.1mm (i.d.);Flowing phase: A
0.1% aqueous formic acid, B methanol, gradient elution program is shown in Table 3;Flow velocity: 0.25mL/min;Sample introduction
Amount: 25 μ L;Column temperature: 30 DEG C.
Table 3
Mass Spectrometry Conditions
Ion source: ESI source;Scan mode: cation scans;Monitoring mode: multiple-reaction monitoring, the most instead
The mass spectrometry parameters optimized under monitoring pattern is answered to be shown in Table 4;Ion transfer tube temperature: 350 DEG C;Sheath gas (High Purity Nitrogen
Gas) 40Arb;Auxiliary gas (high pure nitrogen) 10Arb;Collision gas (high-purity argon gas) 1.5m Torr;Spray voltage:
3Kv。
Table 4
* quota ion is represented
Embodiment 2: the detection of Rynaxypyr residual quantity in Typha latifolia L.
Sample pre-treatments
Weigh 10.00g Typha latifolia L. sample (being accurate to 0.05g) to be placed in tool plug plastic centrifuge tube, add acetic acid second
Ester: acetone (v/v 7: 3) 20mL, ultrasonic 10min, adds the mixing of 3g sodium chloride, and 4000r/min is centrifuged
10min, takes the supernatant and adds 0.1g PSA powder vortex, stand and take 2mL after PSA powder precipitation
The supernatant, is blown to do in 45 DEG C of water-bath rotary evaporations or nitrogen, accurately adds 1.00mL methanol: water mixes
After solution (V/V 3: 7) dissolves, in organic filter membrane of mistake 0.22 μm to sample injection bottle, for Instrumental Analysis.
Chromatogram as shown in Figure 2, liquid phase chromatogram condition is with embodiment 1, and Mass Spectrometry Conditions is with embodiment 1.
Embodiment described above is only to be described the preferred embodiment of the present invention, not to this
Bright scope is defined, under design spirit premise without departing from the present invention, and this area ordinary skill technology people
Member's various deformation of making technical solution of the present invention and improvement, all should fall into claims of the present invention true
In fixed protection domain.
Claims (1)
1. detect a method for Rynaxypyr residual quantity in aquatic vegetable, comprise the steps:
(1) preparation of standard solution:
Accurately weigh 10mg chlorine worm this Methanamide standard substance in 10mL volumetric flask, dissolve constant volume with methanol
To scale, being configured to concentration is 1mg/mL Standard Stock solutions, is placed in-18 DEG C of refrigerators freezing lucifuge and protects
Deposit;
Accurately a certain amount of 1mg/mL Rynaxypyr Standard Stock solutions of absorption is in volumetric flask, uses first
It is 10 μ g/mL intermediate concentration standard solution that alcohol is diluted to mass concentration, is placed in 4 DEG C of refrigerators freezing lucifuge and protects
Deposit;
Accurately draw a certain amount of 10 μ g/mL Rynaxypyr intermediate concentration standard solution, use first respectively
Alcohol and water mixed solution (V/V 3: 7) stepwise dilution are 2ng/mL, 5ng/mL, 10ng/mL to concentration,
The standard working solution of 20ng/mL, 50ng/mL and 100ng/mL, matching while using;
(2) preparation of solvent:
Ethyl acetate: acetone (V/V 7: 3) solvent: measure 700mL ethyl acetate and 300mL acetone,
Mix homogeneously;
Methanol and water mixed solution (V/V 3: 7): measure 300mL methanol and 700mL water, mix homogeneously;
(3) pre-treatment extraction process:
Weigh 10.00g sample (being accurate to 0.05g) to be placed in tool plug plastic centrifuge tube, addition ethyl acetate:
Acetone (v/v 7: 3) 20mL, ultrasonic 10min, add the mixing of 3g sodium chloride, and 4000r/min is centrifuged 10min,
Taking the supernatant and add 0.1g PSA powder vortex, it is clear that standing takes 2mL upper strata after PSA powder precipitation
Liquid, is blown to do in 45 DEG C of water-bath rotary evaporations or nitrogen, accurately adds 1.00mL methanol and water mixed solution
After (V/V 3: 7) dissolves, in organic filter membrane of mistake 0.22 μm to sample injection bottle, for Instrumental Analysis;
(4) measure: take step (1) and filtrate that step (3) obtains carries out liquid chromatography-tandem mass spectrometry
Instrument measures.
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CN104502504A (en) * | 2014-12-30 | 2015-04-08 | 郭庆龙 | Method for measuring residual amount of chlorantraniliprole in vegetables and fruits |
CN104535692A (en) * | 2015-01-19 | 2015-04-22 | 山东出入境检验检疫局检验检疫技术中心 | LC-MS/MS (liquid chromatography-mass spectrometry/mass spectrometry) determination method of residual amount of tetrachlorantraniliprole in fruits and vegetables |
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WO2008096231A1 (en) * | 2007-02-09 | 2008-08-14 | Pfizer Limited | Antiparasitic agents |
CN103512993A (en) * | 2013-10-12 | 2014-01-15 | 崔淑华 | Hot pepper and determining method for 96 pesticide residues in product of hot pepper |
CN104502504A (en) * | 2014-12-30 | 2015-04-08 | 郭庆龙 | Method for measuring residual amount of chlorantraniliprole in vegetables and fruits |
CN104535692A (en) * | 2015-01-19 | 2015-04-22 | 山东出入境检验检疫局检验检疫技术中心 | LC-MS/MS (liquid chromatography-mass spectrometry/mass spectrometry) determination method of residual amount of tetrachlorantraniliprole in fruits and vegetables |
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BALWINDER SINGH 等: "Development and Validation of QuEChERS Method for Estimation of Chlorantraniliprole Residue in Vegetables", 《JOURNAL OF FOOD SCIENCE》 * |
CHRIS SACK 等: "Collaborative Validation of the QuEChERS Procedure for the Determination of Pesticides in Food by LC MS/MS", 《JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY》 * |
ŁUKASZ RAJSKI 等: "Determination of pesticide residues in high oil vegetal commodities by using various multi-residue methods and clean-ups followed by liquid chromatography tandem mass spectrometry", 《JOURNAL OF CHROMATOGRAPHY A》 * |
MAGALI KEMMERICH 等: "Optimization by Central Composite Design of a Modified QuEChERS Method for Extraction of Pesticide Multiresidue in Sweet Pepper and Analysis by Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry", 《FOOD ANAL. METHODS》 * |
张云 等: "液相色谱法测定动物源性食品中氯虫苯甲酰胺和氟虫酰胺残留量", 《分析实验室》 * |
朱建华 等: "液相色谱串联质谱法测定果蔬中的唑虫酰胺、氟啶虫酰胺、氯虫苯甲酰胺及氟虫双酰胺残留", 《分析测试学报》 * |
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