CN111929123A - Pretreatment method for determining carbamate multi-pesticide residues in fruits and vegetables - Google Patents
Pretreatment method for determining carbamate multi-pesticide residues in fruits and vegetables Download PDFInfo
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- 235000012055 fruits and vegetables Nutrition 0.000 title claims abstract description 34
- 239000000447 pesticide residue Substances 0.000 title claims abstract description 27
- 238000002203 pretreatment Methods 0.000 title claims abstract description 16
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 title claims description 15
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 21
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 20
- 239000012629 purifying agent Substances 0.000 claims abstract description 15
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 14
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 12
- 239000006228 supernatant Substances 0.000 claims abstract description 12
- 239000011780 sodium chloride Substances 0.000 claims abstract description 10
- 239000000337 buffer salt Substances 0.000 claims abstract description 9
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 9
- 239000001509 sodium citrate Substances 0.000 claims abstract description 9
- 238000003260 vortexing Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- -1 octadecyl silica gel Chemical compound 0.000 claims description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- 239000000741 silica gel Substances 0.000 claims description 7
- 229910002027 silica gel Inorganic materials 0.000 claims description 7
- 239000000152 carbamate pesticide Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 238000001514 detection method Methods 0.000 abstract description 18
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 150000004657 carbamic acid derivatives Chemical class 0.000 abstract description 2
- 239000000575 pesticide Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 235000013311 vegetables Nutrition 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 240000007124 Brassica oleracea Species 0.000 description 4
- 235000003899 Brassica oleracea var acephala Nutrition 0.000 description 4
- 235000011301 Brassica oleracea var capitata Nutrition 0.000 description 4
- 235000001169 Brassica oleracea var oleracea Nutrition 0.000 description 4
- 238000002137 ultrasound extraction Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- DUEPRVBVGDRKAG-UHFFFAOYSA-N carbofuran Chemical compound CNC(=O)OC1=CC=CC2=C1OC(C)(C)C2 DUEPRVBVGDRKAG-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012224 working solution Substances 0.000 description 2
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- YRRKLBAKDXSTNC-UHFFFAOYSA-N Aldicarb sulfonyl Natural products CNC(=O)ON=CC(C)(C)S(C)(=O)=O YRRKLBAKDXSTNC-UHFFFAOYSA-N 0.000 description 1
- BXPMAGSOWXBZHS-CYBMUJFWSA-N Aldicarb sulphoxide Natural products CNC(=O)ON=CC(C)(C)[S@@](C)=O BXPMAGSOWXBZHS-CYBMUJFWSA-N 0.000 description 1
- YRRKLBAKDXSTNC-WEVVVXLNSA-N Aldoxycarb Chemical compound CNC(=O)O\N=C\C(C)(C)S(C)(=O)=O YRRKLBAKDXSTNC-WEVVVXLNSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 239000005916 Methomyl Substances 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- BXPMAGSOWXBZHS-UITAMQMPSA-N [(z)-(2-methyl-2-methylsulfinylpropylidene)amino] n-methylcarbamate Chemical compound CNC(=O)O\N=C/C(C)(C)S(C)=O BXPMAGSOWXBZHS-UITAMQMPSA-N 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- QGLZXHRNAYXIBU-WEVVVXLNSA-N aldicarb Chemical compound CNC(=O)O\N=C\C(C)(C)SC QGLZXHRNAYXIBU-WEVVVXLNSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- QBSJMKIUCUGGNG-UHFFFAOYSA-N isoprocarb Chemical compound CNC(=O)OC1=CC=CC=C1C(C)C QBSJMKIUCUGGNG-UHFFFAOYSA-N 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- UHXUZOCRWCRNSJ-QPJJXVBHSA-N methomyl Chemical compound CNC(=O)O\N=C(/C)SC UHXUZOCRWCRNSJ-QPJJXVBHSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- 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
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a pretreatment method for determining multi-pesticide residue of carbamates in fruits and vegetables, which comprises the following steps: adding acetonitrile and sodium salt into a fruit and vegetable sample for extraction, adding sulfate, and centrifuging to obtain supernatant; adding the supernatant into a container containing a purifying agent for treatment; the sodium salt comprises sodium citrate buffer salt and sodium chloride, and the mass ratio of the sodium citrate buffer salt to the sodium chloride is 1: 2-10. The invention has the advantages of reducing detection limit, improving sensitivity and anti-interference capability.
Description
Technical Field
The invention relates to the field of pesticide residue analysis in fruits and vegetables. More specifically, the invention relates to a pretreatment method for determining multi-pesticide residue of carbamates in fruits and vegetables.
Background
At present, pesticides are used for preventing and treating plant diseases and insect pests in agricultural production in a large quantity, but the pesticide residue in agricultural products is increased due to unreasonable application of the pesticides. With the increasing level of life and expectation of good life of people, pesticide residue is becoming a concern of people as an important factor influencing the quality and safety of agricultural products and food. The method is very key for detecting pesticide residues in agricultural products in order to effectively prevent the agricultural products with pesticide residues exceeding the standard from entering market channels.
The detection of pesticide residue in agricultural products mainly comprises sample pretreatment and analysis detection. The pretreatment of the sample is used as a key technology for analysis and detection, and the accuracy and reproducibility of an analysis result are directly determined. Meanwhile, the pretreatment of the analysis sample consumes time and labor, comprises the preparation, extraction, separation, purification and the like of the sample, and relates to complex steps, and the high efficiency of the consumption of manpower and material resources is low according to the traditional treatment process. At present, the detection method of the carbamate pesticide residue in food and agricultural products mainly refers to GB 23200.112-2018, but still has a plurality of defects: the pretreatment is complex, and the extraction effect is not good; the detection limit is high, the sensitivity is low, and the increasingly severe requirements are difficult to adapt; the detection result has low reproducibility and weak anti-interference capability.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
The invention also aims to provide a pretreatment method for determining the carbamate multi-pesticide residue in the fruits and vegetables, which adopts the compound sodium salt, the compound sulfate and the compound purifying agent to treat the fruit and vegetable samples, thereby reducing the detection limit, and improving the sensitivity and the anti-interference capability.
To achieve these objects and other advantages in accordance with the present invention, there is provided a pretreatment method for measuring multi-pesticide residues in fruits and vegetables, comprising:
adding acetonitrile and sodium salt into a fruit and vegetable sample for extraction, adding sulfate, and centrifuging to obtain supernatant;
adding the supernatant into a container containing a purifying agent for treatment;
the sodium salt comprises sodium citrate buffer salt and sodium chloride, and the mass ratio of the sodium citrate buffer salt to the sodium chloride is 1: 2-10.
Preferably, the volume ratio of the mass of the fruit and vegetable sample to the acetonitrile is 1 g: 4mL, wherein the mass ratio of the fruit and vegetable sample to the sodium salt is 10: 1-3.
Preferably, the extraction comprises shaking, vortex and ultrasound, the shaking time is 5-10 s, the vortex is completed by adopting a vortex oscillator, the vortex time is 30-40 s, and the ultrasound time is 20-22 min.
Preferably, the sulfate comprises anhydrous sodium sulfate and anhydrous magnesium sulfate, and the mass ratio of the anhydrous sodium sulfate to the anhydrous magnesium sulfate is 1: 3-10.
Preferably, the mass ratio of the fruit and vegetable sample to the sulfate is 10: 1-6.
Preferably, the centrifugation time is 5-6 min, and the centrifugation rotating speed is 4000-4200 r/min.
Preferably, the purifying agent comprises graphitized carbon, ethylenediamine-N-propyl and octadecyl silica gel, and the mass ratio of the graphitized carbon to the ethylenediamine-N-propyl to the octadecyl silica gel is 0.1-1: 0.1-1.
Preferably, the mass ratio of the fruit and vegetable sample to the purifying agent is 10: 1-3.
Preferably, the container is a 50-80 mL centrifuge tube.
Preferably, the treatment is performed by swirling for 30-35 s and then standing for 60-70 s.
The invention at least comprises the following beneficial effects:
the method is simple and quick, and is suitable for the current detection situation;
the treatment effect is good, and the recovery rate is high;
strong practicability, no cross impurity peak and good reproducibility.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
It is to be noted that the experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and the reagents and materials are commercially available unless otherwise specified.
< example 1>
Extraction: weighing 5g of green vegetable leaves (accurate to 0.01g) into a 50mL plastic centrifuge tube, adding 20mL of acetonitrile, adding 0.5g of sodium citrate buffer salt and sodium chloride powder in a mass ratio of 1:2.0, quickly shaking for 5s, then vortexing on a vortexing oscillator for 30s, and ultrasonically extracting for 20 min. An ice bag can be placed in the ultrasonic generator to reduce the temperature generated by the ultrasonic. After the ultrasonic extraction is finished, 0.5g of anhydrous sodium sulfate and anhydrous magnesium sulfate powder in a mass ratio of 1:3.0 are added into the sample extraction solution, the centrifugal tube is manually and violently vibrated to fully disperse the added sulfate, then the centrifugal tube is centrifuged for 5min at 4000r/min, and the supernatant is taken for purification.
Purifying: graphitized Carbon (GCB), ethylenediamine-N-Propyl (PSA) and octadecyl silica gel (C18)1.5g in a mass ratio of 0.1:0.5:1 were placed in a 50mL centrifuge tube. 10mL of supernatant (acetonitrile layer) in the extraction sample centrifuge tube is added into the centrifuge tube filled with the purifying agent. And (4) uniformly mixing for 30s in a vortex manner, and standing for 1min to form a solution to be detected of the pesticide residue in the leaf of the cabbage.
< example 2>
Extraction: weighing 5g of green vegetable leaves (accurate to 0.01g) into a 50mL plastic centrifuge tube, adding 20mL of acetonitrile, adding 1.0g of sodium citrate buffer salt and sodium chloride powder in a mass ratio of 1:10.0, quickly shaking for 10s, then vortexing on a vortexing oscillator for 40s, and ultrasonically extracting for 22 min. An ice bag can be placed in the ultrasonic generator to reduce the temperature generated by the ultrasonic. After the ultrasonic extraction is finished, 1.0g of anhydrous sodium sulfate and anhydrous magnesium sulfate powder in a mass ratio of 1:10.0 are added into the sample extraction solution, the centrifugal tube is manually and violently shaken to fully disperse the added sulfate, then the centrifugal tube is centrifuged for 6min at 4200r/min, and the supernatant is taken and is ready for purification.
Purifying: graphitized Carbon (GCB), ethylenediamine-N-Propyl (PSA) and octadecyl silica gel (C18)0.5g in a mass ratio of 0.5:1.0:0.1 were placed in a 50mL centrifuge tube. 10mL of supernatant (acetonitrile layer) in the extraction sample centrifuge tube is added into the centrifuge tube filled with the purifying agent. And (5) uniformly mixing for 35s in a vortex manner, and standing for 70s to form a solution to be detected of the pesticide residue in the leaf of the cabbage.
< example 3>
Extraction: weighing 5g of green vegetable leaves (accurate to 0.01g) into a 50mL plastic centrifuge tube, adding 20mL of acetonitrile, adding 1.5g of sodium citrate buffer salt and sodium chloride powder in a mass ratio of 1:5.0, quickly shaking for 7s, then vortexing on a vortexing oscillator for 35s, and ultrasonically extracting for 21 min. An ice bag can be placed in the ultrasonic generator to reduce the temperature generated by the ultrasonic. After the ultrasonic extraction is finished, 3.0g of anhydrous sodium sulfate and anhydrous magnesium sulfate powder in a mass ratio of 1:6.0 are added into the sample extraction solution, the centrifugal tube is manually and violently vibrated to fully disperse the added sulfate, then the centrifugal tube is centrifuged at 4100r/min for 6min, and the supernatant is taken for purification.
Purifying: graphitized Carbon (GCB), ethylenediamine-N-Propyl (PSA) and octadecyl silica gel (C18), 1.5g in a mass ratio of 1:0.1:0.5, were placed in a 50mL centrifuge tube. 10mL of supernatant (acetonitrile layer) in the extraction sample centrifuge tube is added into the centrifuge tube filled with the purifying agent. And (4) uniformly mixing for 32s in a vortex manner, and standing for 65s to form a solution to be detected of the pesticide residue in the cabbage leaves.
< example 4>
The treatment method of example 4 was the same as that of example 3 except that 1.0g of anhydrous sodium sulfate and anhydrous magnesium sulfate powder in a mass ratio of 1:4.0 were added to the sample extraction solution, and 1.5g of Graphitized Carbon (GCB), ethylenediamine-N-Propyl (PSA) and octadecylsilicone (C18) in a mass ratio of 0.2:0.6:0.3 were placed in a 50mL centrifuge tube.
< comparative example 1>
The extraction procedure was as in example 1 except that after addition of 20mL of acetonitrile, 0.5g of sodium chloride powder was added.
< comparative example 2>
The extraction procedure was the same as in example 1, except that 0.5g of anhydrous magnesium sulfate powder was added to the sample extraction solution after the completion of the ultrasonic extraction.
< comparative example 3>
The extraction procedure was the same as in example 1 except that in the purification procedure, 1.5g of Graphitized Carbon (GCB) was placed in a 50mL centrifuge tube.
< ion Pair optimization results >
At present, carbamate pesticides are mostly adopted on vegetable leaves, a universal detection method for rapidly determining pesticide residues in vegetables and fruits is established, and 8 carbamate pesticides are selected for detection of the method. In order to obtain higher selectivity and sensitivity, the parent ions, the daughter ions and the collision energy of the pesticide in the LC-MS/MS analysis in the detection method are tested by using a standard solution of the pesticide, and the results are shown in Table 1.
TABLE 1
< detection Limit detection result >
And (3) quantitatively analyzing the liquid to be detected of the separated and extracted cabbage leaf pesticide residue by using a liquid chromatography-mass spectrometer to obtain the content of the carbamate pesticide residue in the fruits and vegetables.
Adding a pesticide standard sample into a to-be-detected solution of the pesticide residue in the vegetable leaves, respectively preparing a series of mixed working solutions with a total concentration of 6 grades of 0.01-5.0 mg/L, and drawing a standard curve by using the concentration-specific component ion peak area; the sample injection concentration is continuously reduced until the peak area is higher than the baseline noise times to be taken as the detection Limit (LOD), and the experimental data of the method detection limit of 8 carbamate pesticides are given in Table 2.
TABLE 2
As can be seen from Table 2, the detection limit of the fruits and vegetables treated by the sodium salt, the sulfate and the purifying agent is lower than that of the fruits and vegetables not treated by the sodium salt, the sulfate and the purifying agent.
< detection of recovery >
Adding a pesticide standard sample into a to-be-detected solution of the pesticide residue in the vegetable leaves, respectively preparing a series of mixed working solutions with a total concentration of 6 grades of 0.01-5.0 mg/L, and drawing a standard curve by using the concentration-specific component ion peak area; adding mixed standard samples with three-level concentrations of 1-2, 0.1-0.2 and 0.01-0.05 into the sample respectively, extracting, purifying, introducing the sample, calculating the recovery rate, and repeating for 3 times. The experimental data for the recovery of 8 carbamate pesticides are given in table 3.
TABLE 3
| Numbering | Name of pesticide | Example 1 | Example 2 | Example 3 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| 1 | Aldicarb | 95.4 | 90.6 | 92.2 | 103.7 | 119.3 | 136.7 | 127.9 |
| 2 | Aldicarb sulfone | 95.1 | 91.7 | 92.3 | 99.8 | 138.3 | 112.0 | 91.5 |
| 3 | Aldicarb sulfoxide | 100.2 | 96.8 | 99.2 | 96.1 | 113.6 | 106.3 | 135.3 |
| 4 | Methomyl | 94.2 | 86.9 | 92.1 | 87.0 | 93.9 | 139.2 | 131.5 |
| 5 | Isoprocarb | 93.2 | 93.7 | 96.3 | 101.0 | 88.0 | 81.4 | 81.1 |
| 6 | Xiweiyin medicine | 92.9 | 103.1 | 102.3 | 102.5 | 136.2 | 82.7 | 79.4 |
| 7 | Carbofuran | 95.0 | 98.7 | 85.2 | 104.9 | 81.4 | 71.1 | 135.8 |
| 8 | Trihydroxy carbofuran | 87.0 | 95.8 | 95.2 | 102.4 | 120.4 | 135.1 | 91.8 |
As can be seen from Table 3, the recovery rates of the fruits and vegetables treated by the sodium salt, the sulfate and the purifying agent are better than those of the fruits and vegetables not treated by the sodium salt, the sulfate and the purifying agent.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the embodiments shown and described without departing from the generic concept as defined by the claims and their equivalents.
Claims (10)
1. A pretreatment method for measuring carbamate multi-pesticide residues in fruits and vegetables is characterized by comprising the following steps:
adding acetonitrile and sodium salt into a fruit and vegetable sample for extraction, adding sulfate, and centrifuging to obtain supernatant;
adding the supernatant into a container containing a purifying agent for treatment;
the sodium salt comprises sodium citrate buffer salt and sodium chloride, and the mass ratio of the sodium citrate buffer salt to the sodium chloride is 1: 2-10.
2. The pretreatment method for measuring the carbamate multi-pesticide residue in the fruits and vegetables according to claim 1, wherein the volume ratio of the mass of the fruit and vegetable sample to the acetonitrile is 1 g: 4mL, wherein the mass ratio of the fruit and vegetable sample to the sodium salt is 10: 1-3.
3. The pretreatment method for measuring the carbamate multi-pesticide residue in the fruits and vegetables according to claim 1, wherein the extraction comprises shaking, vortexing and ultrasound, the shaking time is 5-10 s, the vortexing is completed by a vortexing oscillator, the vortexing time is 30-40 s, and the ultrasound time is 20-22 min.
4. The pretreatment method for measuring the carbamate multi-pesticide residue in the fruits and vegetables according to claim 1, wherein the sulfate comprises anhydrous sodium sulfate and anhydrous magnesium sulfate, and the mass ratio of the anhydrous sodium sulfate to the anhydrous magnesium sulfate is 1: 3-10.
5. The pretreatment method for measuring the carbamate multi-pesticide residue in the fruits and vegetables as claimed in claim 1, wherein the mass ratio of the fruit and vegetable sample to the sulfate is 10: 1-6.
6. The pretreatment method for measuring the carbamate pesticide residue in the fruits and vegetables as claimed in claim 1, wherein the centrifugation time is 5-6 min, and the centrifugation speed is 4000-4200 r/min.
7. The pretreatment method for measuring the carbamate multi-pesticide residue in the fruits and vegetables as claimed in claim 1, wherein the purifying agent comprises graphitized carbon, ethylenediamine-N-propyl and octadecyl silica gel, and the mass ratio of the graphitized carbon, the ethylenediamine-N-propyl and the octadecyl silica gel is 0.1-1: 0.1-1.
8. The pretreatment method for measuring the carbamate multi-pesticide residue in the fruits and vegetables as claimed in claim 1, wherein the mass ratio of the fruit and vegetable sample to the purifying agent is 10: 1-3.
9. The pretreatment method for determining the carbamate multi-pesticide residue in the fruits and vegetables as claimed in claim 1, wherein the container is a 50-80 mL centrifuge tube.
10. The pretreatment method for measuring the carbamate pesticide residue in the fruits and vegetables according to claim 1, wherein the treatment is vortex for 30-35 s and then standing for 60-70 s.
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