CN105675742A - Quantitative detection and rapid pretreatment method of pesticide residues in fruits and vegetables - Google Patents
Quantitative detection and rapid pretreatment method of pesticide residues in fruits and vegetables Download PDFInfo
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- CN105675742A CN105675742A CN201511034649.6A CN201511034649A CN105675742A CN 105675742 A CN105675742 A CN 105675742A CN 201511034649 A CN201511034649 A CN 201511034649A CN 105675742 A CN105675742 A CN 105675742A
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- 238000001514 detection method Methods 0.000 title claims abstract description 15
- 239000000447 pesticide residue Substances 0.000 title claims abstract description 13
- 238000002203 pretreatment Methods 0.000 title claims abstract description 9
- 235000012055 fruits and vegetables Nutrition 0.000 title abstract 2
- 238000012360 testing method Methods 0.000 claims abstract description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000013311 vegetables Nutrition 0.000 claims abstract description 13
- 239000006228 supernatant Substances 0.000 claims abstract description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 239000012528 membrane Substances 0.000 claims abstract description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 5
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 4
- 239000010439 graphite Substances 0.000 claims abstract description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 6
- 239000003242 anti bacterial agent Substances 0.000 claims description 4
- 229940088710 antibiotic agent Drugs 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 239000008346 aqueous phase Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 150000001805 chlorine compounds Chemical class 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 235000013305 food Nutrition 0.000 claims description 3
- 238000005374 membrane filtration Methods 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 9
- 238000005259 measurement Methods 0.000 abstract description 2
- 238000007664 blowing Methods 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 2
- 238000011084 recovery Methods 0.000 description 15
- 240000008067 Cucumis sativus Species 0.000 description 5
- 235000010799 Cucumis sativus var sativus Nutrition 0.000 description 5
- 239000003905 agrochemical Substances 0.000 description 5
- NYPJDWWKZLNGGM-UHFFFAOYSA-N fenvalerate Chemical compound C=1C=C(Cl)C=CC=1C(C(C)C)C(=O)OC(C#N)C(C=1)=CC=CC=1OC1=CC=CC=C1 NYPJDWWKZLNGGM-UHFFFAOYSA-N 0.000 description 4
- 239000002728 pyrethroid Substances 0.000 description 3
- 150000003335 secondary amines Chemical class 0.000 description 2
- WCXDHFDTOYPNIE-RIYZIHGNSA-N (E)-acetamiprid Chemical compound N#C/N=C(\C)N(C)CC1=CC=C(Cl)N=C1 WCXDHFDTOYPNIE-RIYZIHGNSA-N 0.000 description 1
- FSCWZHGZWWDELK-UHFFFAOYSA-N 3-(3,5-dichlorophenyl)-5-ethenyl-5-methyl-2,4-oxazolidinedione Chemical compound O=C1C(C)(C=C)OC(=O)N1C1=CC(Cl)=CC(Cl)=C1 FSCWZHGZWWDELK-UHFFFAOYSA-N 0.000 description 1
- 239000005875 Acetamiprid Substances 0.000 description 1
- 239000005874 Bifenthrin Substances 0.000 description 1
- 239000005944 Chlorpyrifos Substances 0.000 description 1
- 239000005946 Cypermethrin Substances 0.000 description 1
- 239000005892 Deltamethrin Substances 0.000 description 1
- 239000005760 Difenoconazole Substances 0.000 description 1
- FNELVJVBIYMIMC-UHFFFAOYSA-N Ethiprole Chemical compound N1=C(C#N)C(S(=O)CC)=C(N)N1C1=C(Cl)C=C(C(F)(F)F)C=C1Cl FNELVJVBIYMIMC-UHFFFAOYSA-N 0.000 description 1
- 239000005949 Malathion Substances 0.000 description 1
- 239000005663 Pyridaben Substances 0.000 description 1
- YASYVMFAVPKPKE-UHFFFAOYSA-N acephate Chemical compound COP(=O)(SC)NC(C)=O YASYVMFAVPKPKE-UHFFFAOYSA-N 0.000 description 1
- OMFRMAHOUUJSGP-IRHGGOMRSA-N bifenthrin Chemical compound C1=CC=C(C=2C=CC=CC=2)C(C)=C1COC(=O)[C@@H]1[C@H](\C=C(/Cl)C(F)(F)F)C1(C)C OMFRMAHOUUJSGP-IRHGGOMRSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- CRQQGFGUEAVUIL-UHFFFAOYSA-N chlorothalonil Chemical compound ClC1=C(Cl)C(C#N)=C(Cl)C(C#N)=C1Cl CRQQGFGUEAVUIL-UHFFFAOYSA-N 0.000 description 1
- SBPBAQFWLVIOKP-UHFFFAOYSA-N chlorpyrifos Chemical compound CCOP(=S)(OCC)OC1=NC(Cl)=C(Cl)C=C1Cl SBPBAQFWLVIOKP-UHFFFAOYSA-N 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- -1 cyfloxylate Chemical compound 0.000 description 1
- ZXQYGBMAQZUVMI-UNOMPAQXSA-N cyhalothrin Chemical compound CC1(C)C(\C=C(/Cl)C(F)(F)F)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-UNOMPAQXSA-N 0.000 description 1
- 229960005424 cypermethrin Drugs 0.000 description 1
- KAATUXNTWXVJKI-UHFFFAOYSA-N cypermethrin Chemical compound CC1(C)C(C=C(Cl)Cl)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 KAATUXNTWXVJKI-UHFFFAOYSA-N 0.000 description 1
- 229960002483 decamethrin Drugs 0.000 description 1
- OWZREIFADZCYQD-NSHGMRRFSA-N deltamethrin Chemical compound CC1(C)[C@@H](C=C(Br)Br)[C@H]1C(=O)O[C@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 OWZREIFADZCYQD-NSHGMRRFSA-N 0.000 description 1
- JXSJBGJIGXNWCI-UHFFFAOYSA-N diethyl 2-[(dimethoxyphosphorothioyl)thio]succinate Chemical compound CCOC(=O)CC(SP(=S)(OC)OC)C(=O)OCC JXSJBGJIGXNWCI-UHFFFAOYSA-N 0.000 description 1
- BQYJATMQXGBDHF-UHFFFAOYSA-N difenoconazole Chemical compound O1C(C)COC1(C=1C(=CC(OC=2C=CC(Cl)=CC=2)=CC=1)Cl)CN1N=CN=C1 BQYJATMQXGBDHF-UHFFFAOYSA-N 0.000 description 1
- MCWXGJITAZMZEV-UHFFFAOYSA-N dimethoate Chemical compound CNC(=O)CSP(=S)(OC)OC MCWXGJITAZMZEV-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- ZNOLGFHPUIJIMJ-UHFFFAOYSA-N fenitrothion Chemical compound COP(=S)(OC)OC1=CC=C([N+]([O-])=O)C(C)=C1 ZNOLGFHPUIJIMJ-UHFFFAOYSA-N 0.000 description 1
- GBIHOLCMZGAKNG-CGAIIQECSA-N flucythrinate Chemical compound O=C([C@@H](C(C)C)C=1C=CC(OC(F)F)=CC=1)OC(C#N)C(C=1)=CC=CC=1OC1=CC=CC=C1 GBIHOLCMZGAKNG-CGAIIQECSA-N 0.000 description 1
- KVGLBTYUCJYMND-UHFFFAOYSA-N fonofos Chemical compound CCOP(=S)(CC)SC1=CC=CC=C1 KVGLBTYUCJYMND-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- ONUFESLQCSAYKA-UHFFFAOYSA-N iprodione Chemical compound O=C1N(C(=O)NC(C)C)CC(=O)N1C1=CC(Cl)=CC(Cl)=C1 ONUFESLQCSAYKA-UHFFFAOYSA-N 0.000 description 1
- YFVOXLJXJBQDEF-UHFFFAOYSA-N isocarbophos Chemical compound COP(N)(=S)OC1=CC=CC=C1C(=O)OC(C)C YFVOXLJXJBQDEF-UHFFFAOYSA-N 0.000 description 1
- 229960000453 malathion Drugs 0.000 description 1
- NNKVPIKMPCQWCG-UHFFFAOYSA-N methamidophos Chemical compound COP(N)(=O)SC NNKVPIKMPCQWCG-UHFFFAOYSA-N 0.000 description 1
- PZXOQEXFMJCDPG-UHFFFAOYSA-N omethoate Chemical compound CNC(=O)CSP(=O)(OC)OC PZXOQEXFMJCDPG-UHFFFAOYSA-N 0.000 description 1
- LCCNCVORNKJIRZ-UHFFFAOYSA-N parathion Chemical compound CCOP(=S)(OCC)OC1=CC=C([N+]([O-])=O)C=C1 LCCNCVORNKJIRZ-UHFFFAOYSA-N 0.000 description 1
- RLBIQVVOMOPOHC-UHFFFAOYSA-N parathion-methyl Chemical group COP(=S)(OC)OC1=CC=C([N+]([O-])=O)C=C1 RLBIQVVOMOPOHC-UHFFFAOYSA-N 0.000 description 1
- BULVZWIRKLYCBC-UHFFFAOYSA-N phorate Chemical compound CCOP(=S)(OCC)SCSCC BULVZWIRKLYCBC-UHFFFAOYSA-N 0.000 description 1
- QXJKBPAVAHBARF-BETUJISGSA-N procymidone Chemical compound O=C([C@]1(C)C[C@@]1(C1=O)C)N1C1=CC(Cl)=CC(Cl)=C1 QXJKBPAVAHBARF-BETUJISGSA-N 0.000 description 1
- QYMMJNLHFKGANY-UHFFFAOYSA-N profenofos Chemical compound CCCSP(=O)(OCC)OC1=CC=C(Br)C=C1Cl QYMMJNLHFKGANY-UHFFFAOYSA-N 0.000 description 1
- IXTOWLKEARFCCP-UHFFFAOYSA-N propan-2-yl 2-[methoxy-(propan-2-ylamino)phosphinothioyl]oxybenzoate Chemical group CC(C)NP(=S)(OC)OC1=CC=CC=C1C(=O)OC(C)C IXTOWLKEARFCCP-UHFFFAOYSA-N 0.000 description 1
- DWFZBUWUXWZWKD-UHFFFAOYSA-N pyridaben Chemical compound C1=CC(C(C)(C)C)=CC=C1CSC1=C(Cl)C(=O)N(C(C)(C)C)N=C1 DWFZBUWUXWZWKD-UHFFFAOYSA-N 0.000 description 1
- 239000005936 tau-Fluvalinate Substances 0.000 description 1
- INISTDXBRIBGOC-XMMISQBUSA-N tau-fluvalinate Chemical compound N([C@H](C(C)C)C(=O)OC(C#N)C=1C=C(OC=2C=CC=CC=2)C=CC=1)C1=CC=C(C(F)(F)F)C=C1Cl INISTDXBRIBGOC-XMMISQBUSA-N 0.000 description 1
- FFSJPOPLSWBGQY-UHFFFAOYSA-N triazol-4-one Chemical compound O=C1C=NN=N1 FFSJPOPLSWBGQY-UHFFFAOYSA-N 0.000 description 1
- AMFGTOFWMRQMEM-UHFFFAOYSA-N triazophos Chemical compound N1=C(OP(=S)(OCC)OCC)N=CN1C1=CC=CC=C1 AMFGTOFWMRQMEM-UHFFFAOYSA-N 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
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N2030/025—Gas chromatography
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a quantitative detection and rapid pretreatment method of pesticide residues in fruits and vegetables. The method comprises the following steps: 1, preparing a sample; 2, extracting; and 3, purifying: taking 1ml of a supernatant to a small test tube, putting the small test tube in 60DEG C water bath, blowing the supernatant with nitrogen until dryness is nearly reached, adding 1ml of acetone to the blown supernatant to a constant volume, filtering the obtained solution by a 0.22[mu]m filter membrane if the solution is turbid, transferring the solution to a sample bottle, taking the remaining supernatant, filtering the remaining supernatant through a syringe containing 60mg of PSA, 60mg of a graphite carbon core and 200mg of anhydrous magnesium sulfate and provided with the 0.22[mu]m filter membrane, taking 1ml of the above obtained filtrate to a small test tube, putting the small test tube in the 60DEG C water bath, blowing the filtrate with nitrogen until dryness is nearly reached, adding 1ml of n-hexane to a constant volume, and transferring the obtained filtrate to a sample bottle. The pretreatment method has the advantages of simple program and accurate measurement, and can be widely used in quantitative detection of pesticide residues in the vegetables and fruits.
Description
Technical field
The present invention relates to the detection method of a kind of pesticide residue, specifically a kind of vegetables or pesticide residues in fruits detection by quantitative quick pretreatment method.
Background technology
When the many residuals of detection pesticide residues in vegetables medicine, what pre-treating process adopted mostly is the method in NY/T761-2008 standard, this kind of method, measures accurately, but pre-treatment program is complicated, it may also be useful to reagent consumable quantity is big, and cost is higher, is unfavorable for Quick Measurement.
Summary of the invention
It is an object of the invention to provide pesticide residue detection by quantitative quick pretreatment method in the vegetables and fruits that a kind of test processes speed is fast, cost is lower.
The present invention is achieved in that
In vegetables and fruits, pesticide residue detection by quantitative quick pretreatment method, comprises the steps:
Prepared by step one, sample
Choose veterinary antibiotics sample, chopping and fully mixed even after put into food processor and pulverize, be worth treating test sample, put into preservation under-20 DEG C to-16 DEG C conditions, for subsequent use;
Step 2, extraction
Sample 12.0g and treat that test sample is in 50.0ml centrifuge tube, adds 12.0ml trifluoroacetic acid aqueous solution, with 10000r/min homogenate 2min, add anhydrous chlorides of rase sodium 5-8g jolting 1-2min, with the centrifugal 2min of 10000r/min, make acetonitrile phase and aqueous phase layering;
Step 3, purification
Get 1ml supernatant liquor to blow near dry in 60 DEG C of water-bath nitrogen in small test tube, surely hold with 1ml acetone, as muddiness with 0.22 μm of membrane filtration once, go to sample bottle; May be used for the mensuration of FPD organophosphorus parameter.
Supernatant liquor under remainder is with 60mgPSA (primary secondary amine) is housed, 60mg graphite carbon core, the syringe of 200mg anhydrous magnesium sulfate band 0.22 μm of filter membrane filters, and gets 1ml filtrate and blows near dry in 60 DEG C of water-bath nitrogen in small test tube, surely holds with 1ml normal hexane and transfer in sample bottle; May be used for ECD detector and measure organochlorine and pyrethroid intermediate item.
Through the pre-treating process of the present invention, then the conventional means of gas chromatograph detection agricultural chemicals is utilized, just can accurately measure and comprise acephatemet, acephate, omethoate, phorate, Rogor, N-2790, parathion-methyl, fenitrothion 95, Malathion, thiophos, Chlorpyrifos 94, isocarbophos, isofenphos_methyl, Profenofos, triazophos, m-tetrachlorophthalodinitrile, Vinclozoline, RP-26019, triazolone, procymidone, bifenthrin, Fenvalerate, cyhalothrin, pyridaben, cyfloxylate, Cypermethrin, Deltamethrin, taufluvalinate, flucythrinate, fenvalerate, ethiprole, acetamiprid, the residual quantity of difenoconazole totally 33 kinds of agricultural chemicals.The pre-treating process of the present invention, program is simple, measures accurately, it is possible to be widely used in the pesticide residue detection by quantitative of veterinary antibiotics.
Embodiment
In vegetables and fruits, pesticide residue detection by quantitative quick pretreatment method, comprises the steps:
Prepared by step one, sample
Choose veterinary antibiotics sample, chopping and fully mixed even after put into food processor and pulverize, be worth treating test sample, put into preservation under-20 DEG C to-16 DEG C conditions, for subsequent use;
Step 2, extraction
Sample 12.0g and treat that test sample is in 50.0ml centrifuge tube, adds 12.0ml trifluoroacetic acid aqueous solution, with 10000r/min homogenate 2min, add anhydrous chlorides of rase sodium 5 to 8g jolting 1 to 2min, with the centrifugal 2min of 10000r/min, make acetonitrile phase and aqueous phase layering;
Step 3, purification
Get 1ml supernatant liquor to blow near dry in 60 DEG C of water-bath nitrogen in small test tube, surely hold with 1ml acetone, as muddiness with 0.22 μm of membrane filtration once, go to sample bottle; May be used for the mensuration of FPD organophosphorus parameter.
Supernatant liquor under remainder is with 60mgPSA (primary secondary amine) is housed, 60mg graphite carbon core, the syringe of 200mg anhydrous magnesium sulfate band 0.22 μm of filter membrane filters, and gets 1ml filtrate and blows near dry in 60 DEG C of water-bath nitrogen in small test tube, surely holds with 1ml normal hexane and transfer in sample bottle; May be used for ECD detector and measure organochlorine and pyrethroid intermediate item.
Tested by above method and the agricultural chemicals such as organophosphorus, organochlorine and pyrethroid are added in green vegetables and cucumber mark 0.04mg/kg, 0.08mg/kg, the rate of recovery of 0.16mg/kg is respectively: 77.65-102.47%, 77.4-107.76%, 82.44-107.59% and 72.46-105.91%, 78.47-108.53%, 80.47-102.05%; The laboratory variation coefficient exists respectively: 0.5-14.65%, 1.43-19.26%, 1.58-14.17% and 1.81-12.91%, 1.70-17.86%, 0.71-11.71%.
According to GB/T27404-2008, detection method confirms that the tested component concentration of technical requirements and rate of recovery scope are as follows:
It is greater than 100mg/kg, rate of recovery 95-105%,
1-100mg/kg, rate of recovery 90-110%,
0.1-1mg/kg, rate of recovery 80-110%,
It is less than 0.1mg/kg, rate of recovery 60-120%.
The recovery of standard addition of above method is all within the scope of the technical requirements of GB/T27404-2008 detection method confirmation, and 33 kinds of agricultural chemicals all meet pesticide residue and add the rate of recovery requirement marked and reclaim.
Utilize the present invention to measure the recovery testu of 33 kinds of agricultural chemicals in cucumber and green vegetables respectively, obtain experimental data as shown in the table.
Table 1 cucumber adds mark recovery test data: concentration 0.04mg/kg
Table 2 cucumber adds mark recovery test data: concentration 0.08mg/kg
Table 3 cucumber adds mark recovery test data: concentration 0.16mg/kg
Table 4 green vegetables add mark recovery test data: concentration 0.04mg/kg
Table 5 green vegetables add mark recovery test data: concentration 0.08mg/kg
Table 6 green vegetables add mark recovery test data: concentration 0.16mg/kg
Claims (1)
1. pesticide residue detection by quantitative quick pretreatment method in vegetables and fruits, it is characterised in that comprise the steps:
Prepared by step one, sample
Choose veterinary antibiotics sample, chopping and fully mixed even after put into food processor and pulverize, be worth treating test sample, put into preservation under-20 DEG C to-16 DEG C conditions, for subsequent use;
Step 2, extraction
Sample 12.0g and treat that test sample is in 50.0ml centrifuge tube, adds 12.0ml trifluoroacetic acid aqueous solution, with 10000r/min homogenate 2min, add anhydrous chlorides of rase sodium 5 to 8g jolting 1 to 2min, with the centrifugal 2min of 10000r/min, make acetonitrile phase and aqueous phase layering;
Step 3, purification
Get 1ml supernatant liquor in small test tube, blow near dry in 60 DEG C of water-bath nitrogen, surely hold with 1ml acetone, as muddiness with 0.22 μm of membrane filtration once, go to sample bottle;
Supernatant liquor under remainder is with 60mgPSA is housed, and 60mg graphite carbon core, the syringe of 200mg anhydrous magnesium sulfate band 0.22 μm of filter membrane filters, and gets 1ml filtrate in small test tube, blows near dry in 60 DEG C of water-bath nitrogen, surely holds with 1ml normal hexane and transfer in sample bottle.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2015101985908 | 2015-04-19 | ||
| CN201510198590 | 2015-04-19 |
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| Publication Number | Publication Date |
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| CN105675742A true CN105675742A (en) | 2016-06-15 |
| CN105675742B CN105675742B (en) | 2017-11-14 |
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| CN201511034649.6A Expired - Fee Related CN105675742B (en) | 2015-04-19 | 2015-12-27 | Vegetables and fruits Pesticide Residues quantitatively detect quick pretreatment method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107201327A (en) * | 2017-06-02 | 2017-09-26 | 烟台出入境检验检疫局检验检疫技术中心 | One plant of photobacteria and its application in Bravo residue detection |
| CN109725086A (en) * | 2019-03-13 | 2019-05-07 | 盐城市农产品质量监督检验测试中心 | It is a kind of to introduce the residual quick pretreatment method of broken wall treatment detection pesticide residues in vegetables |
| CN110609106A (en) * | 2019-09-16 | 2019-12-24 | 宁波立华制药有限公司 | Method for detecting 11 organophosphorus pesticide residues in white paeony root by using ultra-performance liquid chromatography-mass spectrometry technology |
| CN110824060A (en) * | 2019-11-26 | 2020-02-21 | 江苏韵沣检测有限公司 | Method for determining pesticide residue in vegetables by gas chromatography |
| CN112763734A (en) * | 2021-01-19 | 2021-05-07 | 上海汇像信息技术有限公司 | Pretreatment method for pesticide residue detection |
| CN113325112A (en) * | 2021-06-08 | 2021-08-31 | 贵州茅台酒股份有限公司 | Method for simultaneously and rapidly detecting residual quantity of various pesticides |
| CN113418993A (en) * | 2021-04-07 | 2021-09-21 | 甘肃国信润达分析测试中心 | Method for detecting methyl isosalix phosphorus residue in vegetables and fruits |
| CN114252311A (en) * | 2021-10-27 | 2022-03-29 | 上海市农产品质量安全中心 | Method for carrying out in-situ rapid detection pretreatment on pesticide residues in vegetables and fruits |
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| CN102221589A (en) * | 2011-03-28 | 2011-10-19 | 中国水稻研究所 | Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer |
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| CN109725086A (en) * | 2019-03-13 | 2019-05-07 | 盐城市农产品质量监督检验测试中心 | It is a kind of to introduce the residual quick pretreatment method of broken wall treatment detection pesticide residues in vegetables |
| CN110609106A (en) * | 2019-09-16 | 2019-12-24 | 宁波立华制药有限公司 | Method for detecting 11 organophosphorus pesticide residues in white paeony root by using ultra-performance liquid chromatography-mass spectrometry technology |
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| CN110824060A (en) * | 2019-11-26 | 2020-02-21 | 江苏韵沣检测有限公司 | Method for determining pesticide residue in vegetables by gas chromatography |
| CN112763734A (en) * | 2021-01-19 | 2021-05-07 | 上海汇像信息技术有限公司 | Pretreatment method for pesticide residue detection |
| CN113418993A (en) * | 2021-04-07 | 2021-09-21 | 甘肃国信润达分析测试中心 | Method for detecting methyl isosalix phosphorus residue in vegetables and fruits |
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| CN114252311A (en) * | 2021-10-27 | 2022-03-29 | 上海市农产品质量安全中心 | Method for carrying out in-situ rapid detection pretreatment on pesticide residues in vegetables and fruits |
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