CN109283280B - Method for rapidly extracting and purifying benzoyl urea pesticide residues from fruits and vegetables - Google Patents
Method for rapidly extracting and purifying benzoyl urea pesticide residues from fruits and vegetables Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 26
- HRYILSDLIGTCOP-UHFFFAOYSA-N N-benzoylurea Chemical compound NC(=O)NC(=O)C1=CC=CC=C1 HRYILSDLIGTCOP-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 235000012055 fruits and vegetables Nutrition 0.000 title claims abstract description 22
- 239000000447 pesticide residue Substances 0.000 title claims abstract description 15
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000605 extraction Methods 0.000 claims abstract description 22
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 20
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 19
- 239000006228 supernatant Substances 0.000 claims abstract description 17
- 239000002086 nanomaterial Substances 0.000 claims abstract description 14
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011780 sodium chloride Substances 0.000 claims abstract description 10
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims abstract description 9
- 235000019341 magnesium sulphate Nutrition 0.000 claims abstract description 9
- 239000012528 membrane Substances 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 239000000575 pesticide Substances 0.000 claims description 11
- 235000013399 edible fruits Nutrition 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 235000013311 vegetables Nutrition 0.000 claims description 6
- 239000002917 insecticide Substances 0.000 claims description 4
- 238000001195 ultra high performance liquid chromatography Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 238000000746 purification Methods 0.000 abstract description 10
- 238000001514 detection method Methods 0.000 abstract description 9
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 238000004587 chromatography analysis Methods 0.000 abstract description 3
- 239000000049 pigment Substances 0.000 abstract description 3
- 102000004169 proteins and genes Human genes 0.000 abstract description 3
- 108090000623 proteins and genes Proteins 0.000 abstract description 3
- 235000013305 food Nutrition 0.000 abstract description 2
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 230000005476 size effect Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002949 juvenile hormone Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 239000012224 working solution Substances 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- -1 Transition Metal Disulfide Chemical class 0.000 description 1
- 239000005942 Triflumuron Substances 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000036512 infertility Effects 0.000 description 1
- 230000000749 insecticidal effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000002470 solid-phase micro-extraction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- XAIPTRIXGHTTNT-UHFFFAOYSA-N triflumuron Chemical compound C1=CC(OC(F)(F)F)=CC=C1NC(=O)NC(=O)C1=CC=CC=C1Cl XAIPTRIXGHTTNT-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- 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
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
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- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
- Sampling And Sample Adjustment (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a method for quickly extracting and purifying benzoyl urea pesticide residues from fruits and vegetables, and relates to the technical field of food detection. The detection method comprises the following steps: s1, extraction: weighing the homogenized fruit and vegetable samples into a centrifuge tube, adding acetonitrile for extraction, and then adding sodium chloride and magnesium sulfate to obtain supernatant. S2, purifying: and (3) transferring the supernatant into a centrifugal tube filled with C18 and tungsten disulfide nano materials for purification, and then passing through a 0.22-micron organic microporous filter membrane to obtain a purified solution. And S3, measuring. According to the detection method, an organic solvent acetonitrile is adopted for extraction, sodium chloride and magnesium sulfate are used for dehydration, C18 and tungsten disulfide nano materials are used for purification, and a large amount of pigments in fruits and vegetables or proteins in plant-derived samples can be effectively removed, so that the interference of chromatographic analysis is reduced, and the determination accuracy is improved.
Description
Technical Field
The invention relates to the technical field of food detection, in particular to a method for quickly extracting and purifying benzoyl urea pesticide residues from fruits and vegetables.
Background
Benzoyl urea insecticides, the main component of which is benzoyl urea compounds (BU), are Insect Growth Regulators (IGRs) which can inhibit death or sterility of target pests caused by synthesis of chitin, are known as third-generation insecticides or novel insect control agents, and because of their unique action mechanism, higher environmental safety, broad-spectrum and efficient insecticidal activity and other attractive properties, benzoyl urea compounds have become an active field for creating new pesticides and are widely concerned and applied by people at present.
Even though modern powerful techniques exist for pesticide detection, direct analysis of pesticides is difficult due to the trace level of pesticides in complex environments. Therefore, an enrichment and concentration pre-treatment of the analyte is necessary before the instrumental analysis. Currently, many sample pretreatment techniques are used for extracting pesticides, such as solid-phase extraction, liquid-liquid extraction, solid-phase microextraction, and the like. Among them, solid phase extraction is one of the most effective methods, and has the characteristics of simple operation, short extraction time, good enrichment efficiency, small organic solvent consumption and the like. The QuEChERS extraction separation technology is a rapid sample pretreatment technology for agricultural product detection which is newly developed internationally in recent years, and has the characteristics of high recovery rate, high accuracy and precision, wide analyzable pesticide range, high analysis speed, small solvent usage amount, simple and convenient operation, safety, reliability and the like, so that the QuEChERS extraction separation technology has attracted considerable attention in the field of pesticide detection.
The QuEChERS method generally comprises two steps: firstly, organic solvent extraction and secondly, supernatant purification. The key point of the method is that a dispersive solid-phase extraction (SPE) purification method is adopted, part of extract obtained after the oscillation extraction of an organic solvent is directly added with purification powder for purification, and after centrifugation, the supernatant is taken for instrument analysis. During the QuEChERS extraction process, a large amount of pigment in vegetables and fruits or protein in plant-derived samples can be extracted together with target compounds. These cosolvents may interfere with chromatographic analysis, contaminating the chromatographic column and the ion source. Therefore, the purification of the supernatant by an efficient method is an important factor affecting the detection.
Disclosure of Invention
The invention aims to solve the problems and provide a method for quickly extracting and purifying benzoyl urea pesticide residues from fruits and vegetables, which makes full use of the higher specific surface area, the surface effect, the quantum size effect and the adsorbable effect of a nano material so as to effectively remove impurities and achieve the purification effect and improve the detection sensitivity.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for rapidly extracting and purifying benzoyl urea pesticide residues from fruits and vegetables comprises the following steps:
s1, extraction: weighing the homogenized fruit and vegetable samples into a centrifugal tube, adding acetonitrile, performing vortex extraction for 0.5-2 min, then adding sodium chloride and magnesium sulfate, continuing to perform vortex extraction for 0.5-2 min, and centrifuging at 4000r/min for 2-10 min to obtain a supernatant.
S2, purifying: and transferring the supernatant into a centrifugal tube filled with C18 and tungsten disulfide nano materials, shaking for 1-5 min, centrifuging for 2-10 min at 4000r/min, and then passing through a 0.22-micron organic microporous filter membrane to obtain the purified liquid.
S3, determination: and measuring the concentration of the benzoylurea pesticide in the purified liquid by adopting an ultra-high performance liquid chromatography.
Preferably, in step S1, the fruit or vegetable sample is chopped and then homogenized by a high-pressure homogenizer pump or a high-pressure homogenizer to a particle size of 50 μm or less.
Preferably, in step S1, the mass-to-volume ratio of the homogenized fruit and vegetable sample to acetonitrile is 1-3 g/mL.
Preferably, in step S1, the mass ratio of the sodium chloride to the magnesium sulfate to the homogenized fruit and vegetable samples is 2-5: 10 and 1-3: 10, respectively.
Preferably, in the step S2, the mass-to-volume ratio of the C18 to the supernatant is 20-50 mg/mL; the mass-volume ratio of the tungsten disulfide nano material to the supernatant is 20-50 mg/mL.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1. according to the method for rapidly extracting and purifying the benzoylurea pesticide residues from the fruits and the vegetables, the organic solvent acetonitrile is adopted for extraction, the sodium chloride and the magnesium sulfate are used for removing water, and the C18 and the tungsten disulfide nano material are evolved, so that a large amount of pigments in the fruits and the vegetables or proteins in plant-derived samples can be effectively removed, the interference of chromatographic analysis is reduced, and the determination accuracy is improved.
2. The invention relates to a method for quickly extracting and purifying benzoyl urea pesticide residues from fruits and vegetables, which adopts C18 and tungsten disulfide as purification fillers, and tungsten disulfide (WS)2) The nano material is an important Transition Metal Disulfide (TMDs), has a layered structure similar to graphene, is large in specific surface area and adjustable in band gap, has a unique two-dimensional nano structure, has the characteristics of a nano tube and activated carbon, is insoluble in acid, alkali and alcohol, and has certain reducibility; due to the high specific surface area, the surface effect, the quantum size effect and the small size effect, the method and the C18 have the combined action, so that the initial degree of the purified liquid can be improved, the interference is reduced, and the determination accuracy is improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
First, related reagent material
Sodium chloride (analytical grade, chemical reagents of the national drug group, Shanghai Co., Ltd.); anhydrous magnesium sulfate (analytically pure, shinny and Fine chemical research institute in Tianjin); octadecyl bonded phase silica gel (C18) scavenger (beijing yoxiang technologies ltd); tungsten disulfide nanomaterial (Nanjing pioneer nanomaterial science and technology Co., Ltd.).
Example 1
A method for rapidly extracting and purifying benzoyl urea pesticide residues from fruits and vegetables comprises the following steps:
s1, extraction: weighing 10g of homogenized fruit and vegetable samples into a centrifuge tube, adding 20mL of acetonitrile, performing vortex extraction for 0.5-2 min, then adding 3g of sodium chloride and 2g of magnesium sulfate, continuing to perform vortex extraction for 0.5-2 min, and performing centrifugation for 2-10 min at 4000r/min to obtain a supernatant.
S2, purifying: and transferring the 2ml of supernatant into a centrifugal tube filled with 50mg of C18 and 50mg of tungsten disulfide nano material, shaking for 1-5 min, centrifuging for 2-10 min at 4000r/min, and then passing through a 0.22-micron organic microporous filter membrane to obtain the purified solution.
S3, determination: and measuring the concentration of the benzoylurea pesticide in the purified liquid by adopting an ultra-high performance liquid chromatography.
Example 2
A method for rapidly extracting and purifying benzoyl urea pesticide residues from fruits and vegetables comprises the following steps:
s1, extraction: cutting fruit and vegetable samples, and homogenizing with high pressure homogenizer pump or high pressure homogenizer to obtain particle size below 50 μm. Weighing 10g of homogenized fruit and vegetable samples into a centrifuge tube, adding 15mL of acetonitrile, performing vortex extraction for 0.5-2 min, then adding 4g of sodium chloride and 3g of magnesium sulfate, continuing to perform vortex extraction for 0.5-2 min, and performing centrifugation for 2-10 min at 4000r/min to obtain a supernatant.
S2, purifying: and transferring the 2ml of supernatant into a centrifugal tube filled with 40mg of C18 and 60mg of tungsten disulfide nano material, shaking for 1-5 min, centrifuging for 2-10 min at 4000r/min, and then passing through a 0.22-micron organic microporous filter membrane to obtain the purified solution.
S3, determination: and measuring the concentration of the benzoylurea pesticide in the purified liquid by adopting an ultra-high performance liquid chromatography.
Comparative example 1
Compared with the method in the example 1, in the step S2, 2ml of supernate is taken and transferred to a centrifuge tube filled with 100mg of C18 for experiment, and other steps are the same.
Comparative example 2
Compared with the method in the example 1, in the step S2, 2ml of supernate is taken and transferred to a centrifuge tube filled with 50mg of C18 and 50mg of activated carbon for experiment, and other steps are the same.
Examples of the experiments
(1) Preparation of standard solution: preparation of 100mg L concentration using chromatographic grade methanol-1And then stored at 5 ℃ prior to use. The working solution was prepared by diluting the stock solution with methanol.
(2) The standard solution was diluted with methanol to working solutions of different concentrations (5. mu.g kg-1～2000μg kg-1) Then, the measurement was carried out: each concentration was assayed in duplicate 3 times to obtain the linear equation and correlation coefficient for triflumuron.
(3) The methods for rapidly extracting and purifying the benzoyl urea pesticide residues of example 1, example 2, comparative example 1 and comparative example 2 were respectively adopted for extraction, purification and measurement, and the average recovery rate and RSD were calculated and shown in Table 1.
TABLE 1 analysis of the results
| Measurement method | Example 1 | Example 2 | Comparative example 1 | Comparative example 2 |
| Percent recovery% | 96 | 93 | 95 | 88 |
| RSD/% (day n ═ 3) | 4.6 | 4.7 | 6.8 | 6.2 |
As can be seen from the examples 1-2, the comparative examples 1-2 and the experimental examples, the method for quickly extracting and purifying the benzoylurea pesticide residues from the fruits and the vegetables can accurately and quickly measure the benzoylurea pesticide residues.
The above description is directed to the details of the preferred and possible embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention. All changes, modifications and variations that are equivalent to those made by the technical idea presented in the invention shall fall within the scope of the invention.
Claims (4)
1. A method for rapidly extracting and purifying benzoyl urea pesticide residues from fruits and vegetables is characterized by comprising the following steps:
s1, extraction: weighing homogenized fruit and vegetable samples into a centrifugal tube, adding acetonitrile, performing vortex extraction for 0.5-2 min, then adding sodium chloride and magnesium sulfate, continuing to perform vortex extraction for 0.5-2 min, and centrifuging at 4000r/min for 2-10 min to obtain a supernatant;
s2, purifying: transferring the supernatant into a centrifugal tube filled with C18 and tungsten disulfide nano materials, shaking for 1-5 min, centrifuging for 2-10 min at 4000r/min, and then passing through a 0.22 mu m organic microporous filter membrane to obtain a purified solution;
the mass-volume ratio of the C18 to the supernatant is 20-50 mg/mL; the mass-volume ratio of the tungsten disulfide nano material to the supernatant is 20-50 mg/mL;
s3, determination: and measuring the concentration of the benzoylurea pesticide in the purified liquid by adopting an ultra-high performance liquid chromatography.
2. The method for rapidly extracting and purifying benzoylurea insecticides as claimed in claim 1, wherein in step S1, the fruit or vegetable is cut into pieces, and then homogenized with a high pressure homogenizer pump or a high pressure homogenizer to a particle size of 50 μm or less.
3. The method for rapidly extracting and purifying benzoylurea pesticide residues from fruits and vegetables according to claim 1, wherein in step S1, the mass-to-volume ratio of the homogenized fruit and vegetable sample to acetonitrile is 1-3 g/mL.
4. The method for rapidly extracting and purifying benzoylurea insecticides as claimed in claim 1, wherein the mass ratio of sodium chloride and magnesium sulfate to the homogenized fruit and vegetable samples in step S1 is 2-5: 10 and 1-3: 10 respectively.
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| CN111929123A (en) * | 2020-07-07 | 2020-11-13 | 武汉市农业科学院 | Pretreatment method for determining carbamate multi-pesticide residues in fruits and vegetables |
| CN112844343A (en) * | 2020-12-28 | 2021-05-28 | 江西省食品检验检测研究院（江西国家果蔬产品及加工食品质量监督检验中心） | Quick purge tube of pesticide residue in fruit vegetables |
| CN113514302A (en) * | 2021-07-13 | 2021-10-19 | 湖北琪谱检测技术有限公司 | Efficient pretreatment method for pesticide residue detection sample |
| CN113933443B (en) * | 2021-10-27 | 2024-05-03 | 上海市农产品质量安全中心 | In-situ rapid detection method for acetamiprid in vegetables or fruits |
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