CN110749672A - Method for detecting picoxystrobin residue in bananas - Google Patents
Method for detecting picoxystrobin residue in bananas Download PDFInfo
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- CN110749672A CN110749672A CN201911016752.6A CN201911016752A CN110749672A CN 110749672 A CN110749672 A CN 110749672A CN 201911016752 A CN201911016752 A CN 201911016752A CN 110749672 A CN110749672 A CN 110749672A
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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
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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
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- G—PHYSICS
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- 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
- G01N30/48—Sorbent materials therefor
- G01N30/482—Solid sorbents
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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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
- G01N2030/062—Preparation extracting sample from raw material
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N2030/645—Electrical detectors electrical conductivity detectors
Abstract
The invention discloses a method for detecting picoxystrobin residue in bananas, belonging to the technical field of pesticide residue detection. The detection method comprises the following steps: extracting, purifying and analyzing, wherein the analyzing and measuring parameters are as follows: HP-5(30 m.times.320. mu.m.times.0.25 μm); sample inlet temperature: 250 ℃; detector temperature: 280 ℃; temperature rising procedure: maintaining at 100 deg.C for 1min, and increasing to 260 deg.C at 30 deg.C/min for 5 min; column flow rate: 1 mL/min; sample introduction amount: 1.0. mu.L. The detection method has the advantages of high sensitivity, accuracy, reliability and simplicity in operation, and can detect picoxystrobin residues in bananas in a short time. The lowest detection amount of picoxystrobin in the banana by the method is 0.01 mu g.
Description
Technical Field
The invention belongs to the technical field of pesticide residue detection, and particularly relates to a method for detecting picoxystrobin residue in bananas.
Background
The picoxystrobin is a strobilurin fungicide with a good using effect on bananas at present, is used for preventing and treating sigatoka and the like, and can cause pesticide residues when being used, the maximum residue limit of picoxystrobin on bananas and the international standard of a detection method are not established in China at present, the maximum residue limit of picoxystrobin on bananas is also not established by the international food law committee, and the maximum residue limit of picoxystrobin on bananas is established in the UK to be 0.05 mg/kg. Therefore, a method for detecting picoxystrobin residue in bananas is needed to be established, and the method has important significance for detecting picoxystrobin residue in bananas and ensuring the edible safety of bananas.
National international standard of the picoxystrobin detection method on bananas is not established, and according to the reference literature, some researchers develop the detection technology of picoxystrobin in other substrates, but no relevant report about the picoxystrobin detection method in bananas exists, and the requirements of different substrates on the detection method are essentially different, especially in the extraction and purification links.
Therefore, the method has important significance in the research of the detection method of picoxystrobin in bananas.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a method for detecting picoxystrobin residues in bananas, which is high in sensitivity, accurate, reliable and simple to operate.
The invention adopts the following technical scheme:
the invention provides a method for detecting picoxystrobin residue in bananas, which comprises the following steps:
step one, extraction: adding acetonitrile into a banana sample, mixing and extracting, centrifuging, taking supernatant, adding sodium chloride into the supernatant, shaking, standing to take the supernatant, and concentrating to obtain a solution to be purified;
step two, purification: pre-leaching the solid phase extraction column with mixed solution of n-hexane and acetone, and n-hexane respectively, discarding eluate, immediately pouring into solution to be purified, collecting purified solution, concentrating under reduced pressure to dry, fixing volume, and detecting by gas chromatography;
step three, analysis and determination:
a chromatographic column: HP-5(30 m.times.320. mu.m.times.0.25 μm);
sample inlet temperature: 250 ℃; detector temperature: 280 ℃;
temperature rising procedure: maintaining at 100 deg.C for 1min, and increasing to 260 deg.C at 30 deg.C/min for 5 min;
column flow rate: 1 mL/min;
sample introduction amount: 1.0. mu.L.
In some of these embodiments, the mixing extraction of step one is vortex mixing extraction with an extraction time of 2.0 min.
In some embodiments, the rotation speed of the centrifugation in the first step is 4000r/min, and the centrifugation time is 5 min.
In some embodiments, the mixed solution of n-hexane and acetone in the second step is obtained by mixing n-hexane and acetone according to a volume ratio of 9: 1.
In some embodiments, when the solid-phase extraction column is pre-poured in the second step, the volume ratio of the mixed solution of n-hexane and acetone to n-hexane is 1: 1.
In some embodiments, the solid phase extraction column in step two is a dispersion purification of ethylenediamine-N-propylsilane and octadecylsilane bonded phase matrix.
In some of these embodiments, the banana samples in step one are banana whole fruit and banana pulp samples that are pre-treated to be concentrated by a factor of 3.5 prior to the assay.
In the invention, picoxystrobin is a polar compound, and all organic solvents are selected according to the similar compatibility principle. Polar organic solvent is selected to extract picoxystrobin in the bananas, and the extraction efficiency of acetonitrile is found to be higher by comparing acetone, acetonitrile and ethanol; in the research of the purification process, n-hexane is found: the acetone (9:1) is more beneficial to the separation of picoxystrobin and impurities; the solid-phase extraction column (dispersion and purification of matrix of ethylenediamine-N-Propyl Silane (PSA) and octadecylsilane bonded phase (C18)) is adopted to facilitate the separation of picoxystrobin and impurities. The chemical solvent is effectively selected through the processes of extraction, separation, purification and the like, so that the average recovery rate of the final detection method reaches 101.4-109.2%, and the RSD value is 2.51-3.99%. Is the key of the detection method of the invention.
Compared with the prior art, the invention has the beneficial effects that:
the picoxystrobin residual in the banana sample is extracted by acetonitrile or an acetonitrile solution containing sodium chloride, and the extract is detected by a gas chromatography ECD after being dispersed and purified by ethylenediamine-N-Propyl Silane (PSA) and octadecylsilane bonded phase (C18) matrixes.
The detection method has the advantages of high sensitivity, accuracy, reliability and simplicity in operation, and can detect picoxystrobin residues in bananas in a short time. The method has the advantages that the lowest detection amount of picoxystrobin in the bananas is 0.01 mu g, and the lowest detection concentrations of picoxystrobin in whole bananas, banana pulp and soil samples are 0.02mg/kg, 0.02mg/kg and 0.01mg/kg respectively. The method has higher reference value for formulating the picoxystrobin residue detection method in bananas, and is suitable for popularization and application.
Drawings
FIG. 1 is a chromatogram of picoxystrobin in a banana sample in example 1 of the invention;
FIG. 2 is a standard curve of picoxystrobin.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, which is defined in the appended claims, as may be amended by those skilled in the art upon reading the present invention.
The invention provides a method for detecting picoxystrobin residue in bananas, which comprises the following steps:
step one, extraction: adding acetonitrile into a banana sample, mixing and extracting, centrifuging, taking supernatant, adding sodium chloride into the supernatant, shaking, standing to take the supernatant, and concentrating to obtain a solution to be purified;
step two, purification: pre-leaching the solid phase extraction column with mixed solution of n-hexane and acetone, and n-hexane respectively, discarding eluate, immediately pouring into solution to be purified, collecting purified solution, concentrating under reduced pressure to dry, fixing volume, and detecting by gas chromatography;
step three, analysis and determination:
a chromatographic column: HP-5(30 m.times.320. mu.m.times.0.25 μm);
sample inlet temperature: 250 ℃; detector temperature: 280 ℃;
temperature rising procedure: maintaining at 100 deg.C for 1min, and increasing to 260 deg.C at 30 deg.C/min for 5 min;
column flow rate: 1 mL/min;
sample introduction amount: 1.0. mu.L.
In one embodiment, the mixed extraction of step one is vortex mixed extraction, and the extraction time is 2.0 min.
In one embodiment, the rotation speed of the centrifugation in the first step is 4000r/min, and the centrifugation time is 5 min.
In one embodiment, the mixed solution of n-hexane and acetone in the second step is obtained by mixing n-hexane and acetone according to a volume ratio of 9: 1.
In one embodiment, when the solid-phase extraction column is pre-poured in the second step, the volume ratio of the mixed solution of n-hexane and acetone to n-hexane is 1: 1.
In one embodiment, the solid phase extraction column in the second step is used for matrix dispersion purification of the bonding phase of ethylenediamine-N-propylsilane and octadecylsilane.
In one embodiment, the banana samples in step one are whole banana fruit and banana pulp samples, which are pre-treated to be concentrated by a factor of 3.5 before the assay.
The present invention will be described in detail with reference to specific examples.
Example 1
(1) Extraction of
Weighing 20.0 +/-0.1 g of banana sample into a 50mL centrifuge tube, adding 40mL of acetonitrile, extracting for 2.0min by using a vortex mixer, centrifuging for 5min at 4000r/min, transferring the supernatant into a measuring cylinder with a plug containing 5.0-7.0 g of sodium chloride, violently shaking for 2min, standing for 30min, taking 20mL of the supernatant, concentrating to about 2mL, and purifying.
The pretreatment of the banana whole fruit and banana pulp samples is concentrated by 3.5 times, and the rest samples are unchanged.
(2) Purification
A10 mL disposable syringe tube was taken, 50mg of ethylenediamine-N-Propylsilane (PSA) and 100mg of octadecylsilane chemically bonded phase (C18) were added, 5mL of N-hexane: acetone (9:1, V/V) was used for pre-leaching, and 5mL of N-hexane was used for leaching the solid phase extraction column. The leacheate was discarded and the solution to be purified was immediately poured in and collected in a 100mL round bottom flask. Washing the residue in the round-bottom flask with 5mL of n-hexane/acetone (9:1, V/V), washing the solid phase extraction column with water, repeating the steps for three times, concentrating the collected liquid under reduced pressure (40 ℃) until the collected liquid is dry, fixing the volume with 2.0mL of n-hexane, and detecting by a gas chromatograph.
(3) Analytical determination
A chromatographic column: HP-5(30 m.times.320. mu.m.times.0.25 μm);
sample inlet temperature: 250 ℃; detector temperature: 280 ℃;
temperature rising procedure: maintaining at 100 deg.C for 1min, and increasing to 260 deg.C at 30 deg.C/min for 5 min;
column flow rate: 1 mL/min;
sample introduction amount: 1.0. mu.L.
Under the chromatographic conditions, the retention time of picoxystrobin is about 8.4min respectively.
The instrument conditions were as follows:
a chromatographic column: HP-5(30 m.times.320. mu.m.times.0.25 μm);
sample inlet temperature: 250 ℃; detector temperature: 280 ℃;
temperature rising procedure: maintaining at 100 deg.C for 1min, and increasing to 260 deg.C at 30 deg.C/min for 5 min;
column flow rate: 1 mL/min;
sample introduction amount: 1.0 μ L;
standard curve: weighing picoxystrobin standard substance, dissolving the picoxystrobin standard substance by using n-hexane to prepare mother solution, transferring a proper amount of mother solution to a volumetric flask, diluting the mother solution by using n-hexane to obtain series of standard solutions with mass concentrations of 0.005, 0.01, 0.05, 0.1, 0.5 and 1.0 mu g/mL, respectively, measuring under the conditions of the instrument, and respectively taking the concentration and peak area of the picoxystrobin standard solution as standard curves. The linear equation is: y is 38811x-101.23, and the correlation coefficient is: r2 ═ 0.9997; wherein y is the peak area and x is the standard solution concentration.
TABLE 1 picoxystrobin Standard Curve
TABLE 2 recovery rate of picoxystrobin addition in banana
The embodiments of the present invention have been described in detail with reference to the above examples, but the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (7)
1. The method for detecting picoxystrobin residue in bananas is characterized by comprising the following steps:
step one, extraction: adding acetonitrile into a banana sample, mixing and extracting, centrifuging, taking supernatant, adding sodium chloride into the supernatant, shaking, standing to take the supernatant, and concentrating to obtain a solution to be purified;
step two, purification: pre-leaching the solid phase extraction column with mixed solution of n-hexane and acetone, and n-hexane respectively, discarding eluate, immediately pouring into solution to be purified, collecting purified solution, concentrating under reduced pressure to dry, fixing volume, and detecting by gas chromatography;
step three, analysis and determination:
a chromatographic column: HP-5(30 m.times.320. mu.m.times.0.25 μm);
sample inlet temperature: 250 ℃; detector temperature: 280 ℃;
temperature rising procedure: maintaining at 100 deg.C for 1min, and increasing to 260 deg.C at 30 deg.C/min for 5 min;
column flow rate: 1 mL/min;
sample introduction amount: 1.0. mu.L.
2. The method for detecting picoxystrobin residues in bananas according to claim 1, wherein the mixed extraction in the first step is vortex mixed extraction, and the extraction time is 2.0 min.
3. The method for detecting picoxystrobin residues in bananas according to claim 1, wherein the rotation speed in the centrifugation in the first step is 4000r/min, and the centrifugation time is 5 min.
4. The method for detecting picoxystrobin residue in bananas according to claim 1, wherein the mixed solution of n-hexane and acetone in the second step is obtained by mixing n-hexane and acetone according to a volume ratio of 9: 1.
5. The method for detecting picoxystrobin residue in bananas according to claim 4, wherein when the solid-phase extraction column is pre-sprayed in the second step, the volume ratio of the mixed solution of n-hexane and acetone to n-hexane is 1: 1.
6. The method for detecting picoxystrobin residues in bananas according to claim 4, wherein the solid phase extraction column in the second step is dispersion purification of ethylenediamine-N-propyl silane and octadecylsilane bonded phase matrix.
7. The method according to claim 1, wherein the banana sample in the first step is a whole banana fruit and banana pulp sample, and the whole banana fruit and banana pulp sample is pre-treated and concentrated by 3.5 times before measurement.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| WO2017162801A1 (en) * | 2016-03-23 | 2017-09-28 | Anaquant | Soluble balls for preparing solutions |
| CN108896694A (en) * | 2018-07-05 | 2018-11-27 | 中国农业科学院农业质量标准与检测技术研究所 | A kind of remaining LC-QToF-MS Screening analysis method of pesticide in animal food |
| CN109254099A (en) * | 2018-11-30 | 2019-01-22 | 中国测试技术研究院 | The gas chromatography-mass spectrum rapid assay methods of non-registration ingredient in pesticidal preparations |
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2019
- 2019-10-24 CN CN201911016752.6A patent/CN110749672A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015121802A1 (en) * | 2014-02-12 | 2015-08-20 | Isagro S.P.A. | Benzoylphenyl-formamidines having a fungicidal activity, their agronomic compositions and relative use |
| WO2017162801A1 (en) * | 2016-03-23 | 2017-09-28 | Anaquant | Soluble balls for preparing solutions |
| CN108896694A (en) * | 2018-07-05 | 2018-11-27 | 中国农业科学院农业质量标准与检测技术研究所 | A kind of remaining LC-QToF-MS Screening analysis method of pesticide in animal food |
| CN109254099A (en) * | 2018-11-30 | 2019-01-22 | 中国测试技术研究院 | The gas chromatography-mass spectrum rapid assay methods of non-registration ingredient in pesticidal preparations |
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| Title |
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| BOŻENA ŁOZOWICKA 等: "Occurrence of pesticide residues in fruit from Podlasie (Poland) in 2012", 《JOURNAL OF PLANT PROTECTION RESEARCH》 * |
| JUNG-AH DO 等: "Development and Validation of Analytical Methods for Picoxystrobin Determination in Agricultural Products by GC-ECD and GC-MS", 《J. FD HYG. SAFETY》 * |
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