CN110824060A - Method for determining pesticide residue in vegetables by gas chromatography - Google Patents
Method for determining pesticide residue in vegetables by gas chromatography Download PDFInfo
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- CN110824060A CN110824060A CN201911174835.8A CN201911174835A CN110824060A CN 110824060 A CN110824060 A CN 110824060A CN 201911174835 A CN201911174835 A CN 201911174835A CN 110824060 A CN110824060 A CN 110824060A
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/14—Preparation by elimination of some components
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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
- G01N30/70—Electron capture 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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
Abstract
The invention discloses a method for determining pesticide residues in vegetables by gas chromatography, which comprises the following steps: pretreating a sample, namely taking 15.00g of a homogeneous sample to be detected into a 200mL flask, adding 15mL of acetonitrile, homogenizing for 90s by using a high-speed homogenizer, filtering into a measuring cylinder with a plug, which is pre-filled with 5g of sodium chloride, fully shaking up, and standing for 25 min; transferring 15mL of supernatant into a small beaker, adding about 8g of anhydrous sodium sulfate, and uniformly mixing; purifying, performing vortex on a vortex mixer for 10min, centrifuging at 4000r/min for 5min, collecting acetonitrile solution, adding 5mL acetonitrile, repeatedly extracting, diluting acetone to 2mL, and purifying with a QuEChERS purification tube; gas detection of a gas chromatograph; and (5) detecting the recovery rate and analyzing the result. The invention properly concentrates the extracting solution and then carries out purification treatment so as to improve the detection sensitivity of the method. The method has the advantages of reducing the consumption of the solvent, saving time, being suitable for quickly screening the residual pesticides in the vegetable sample, having higher detection effectiveness and being worthy of popularization and application.
Description
Technical Field
The invention belongs to the field of detection, and particularly relates to a method for determining pesticide residues in vegetables by using a gas chromatography.
Background
The development of agricultural industrialization makes the production of agricultural products depend on exogenous substances such as pesticides, antibiotics and hormones. The amount of agricultural chemicals in agricultural products in China is high, and the unreasonable use of the substances can lead to the overproof pesticide residues in the agricultural products, influence the edible safety of consumers, and cause the consumers to have diseases and abnormal development in serious cases, even directly cause poisoning and death. The over-standard pesticide residue also affects the trade of agricultural products, countries in the world pay high attention to the problem of pesticide residue, and increasingly strict limit standards are stipulated for pesticide residue in various agricultural and sideline products, so that the export of agricultural products in China faces a severe challenge. The design of a convenient, sensitive and accurate pesticide residue detection method becomes a problem to be solved urgently for realizing the safety supervision of vegetables.
Disclosure of Invention
The invention aims to provide a method for measuring pesticide residue in vegetables by using a gas chromatography, which is used for rapidly screening pesticide residue in vegetable samples by using the gas chromatography and improving the sensitivity and precision of detection.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for measuring pesticide residue in vegetables by gas chromatography comprises the following steps:
s1, pre-treating a sample,
fully crushing and uniformly mixing a vegetable sample by using a food processor to prepare a uniform sample to be detected, weighing 15.00g of the uniform sample to be detected in a 200mL flask, adding 15mL of acetonitrile, homogenizing for 90s by using a high-speed homogenizer, filtering into a measuring cylinder with a plug, fully shaking, and standing for 25min, wherein 5g of sodium chloride is placed in the measuring cylinder in advance; transferring 15mL of supernatant into a small beaker, adding about 8g of anhydrous sodium sulfate, and uniformly mixing;
s2, purifying the waste water,
adding the uniformly mixed solution into a centrifuge tube, carrying out vortex on a vortex mixer for 10min, centrifuging for 5min at 4000r/min, collecting acetonitrile solution to a concentration bottle, adding 5mL of acetonitrile for repeated extraction, combining extracting solutions, carrying out nitrogen blowing concentration to a constant volume of 5mL, accurately taking out 2mL of the acetonitrile solution, blowing the nitrogen to near dryness, carrying out acetone constant volume to 2mL, purifying by a QuEChERS purification tube, and carrying out high-speed centrifugation to obtain a supernatant;
s3, detecting the gas phase,
working conditions of the gas chromatograph: no split sample inlet, sample inlet temperature: 280 ℃; ECD detector temperature: 300 ℃; the column temperature procedure was: heating to 220 deg.C for 10min, and heating to 300 deg.C at 30 deg.C/min (maintaining for 15 min); carrier gas: is high-purity nitrogen; sample introduction amount: 1 μ L.
S4, detecting the recovery rate,
taking green vegetables as samples to perform recovery rate tests of 3 concentrations of dimethoate, omethoate, chlorpyrifos and phorate solution, repeating the tests for 3 times, and determining the accuracy and precision of the method; meanwhile, according to the pretreatment procedure of the method, 9 common pesticides such as cypermethrin and the like are selected, and when the addition concentration is 0.1mg/kg, the addition recovery rate test of hot pepper, quintozene, vinclozolin, chlorothalonil, triadimefon, dicofol, procymidone, bifenthrin and fenpropathrin is carried out, and the applicability of the method to the common pesticides is examined.
S5, analyzing the result,
selecting low, medium and high 3 concentrations in the linear range of the working curve, taking the signal-to-noise ratio of a chromatographic peak of the compound to be detected equal to 3 as the detection limit of the method, and taking the mass concentration corresponding to S/N (S/N) 10 as the quantification limit of the method.
Further, S3, a gas chromatograph for gas phase detection adopts a GC-6820 model of Agilent company in America, an Electron Capture Detector (ECD), and a chromatographic column adopts a ZB-50 model with the specification of 30mx0.53mmx0.25 mu m;
further, s3. nitrogen purity in gas phase detection: 99.999 percent.
The invention has the beneficial effects that:
the invention uses gas chromatography to detect pesticide residue in vegetables. The method has the advantages of simple and convenient operation, high sensitivity, good accuracy and the like. The extracting solution is properly concentrated and then is purified, so that the detection sensitivity of the method is improved. The method has the advantages of reducing the consumption of the solvent, saving time, being suitable for quickly screening the residual pesticides in the vegetable sample, having higher detection effectiveness and being worthy of popularization and application.
Drawings
FIG. 1 is a schematic flow chart of a method for measuring pesticide residues in vegetables by using gas chromatography according to the invention;
Detailed Description
The details of the present invention are described below with reference to the accompanying drawings and specific embodiments.
As shown in fig. 1, a method for measuring pesticide residue in vegetables by gas chromatography comprises the following steps:
s1, pre-treating a sample,
fully crushing and uniformly mixing a vegetable sample by using a food processor to prepare a uniform sample to be detected, weighing 15.00g of the uniform sample to be detected in a 200mL flask, adding 15mL of acetonitrile, homogenizing for 90s by using a high-speed homogenizer, filtering into a measuring cylinder with a plug, fully shaking, and standing for 25min, wherein 5g of sodium chloride is placed in the measuring cylinder in advance; transferring 15mL of supernatant into a small beaker, adding about 8g of anhydrous sodium sulfate, and uniformly mixing;
s2, purifying the waste water,
adding the uniformly mixed solution into a centrifuge tube, carrying out vortex on a vortex mixer for 10min, centrifuging for 5min at 4000r/min, collecting acetonitrile solution to a concentration bottle, adding 5mL of acetonitrile for repeated extraction, combining extracting solutions, carrying out nitrogen blowing concentration to a constant volume of 5mL, accurately taking out 2mL of the acetonitrile solution, blowing the nitrogen to near dryness, carrying out acetone constant volume to 2mL, purifying by a QuEChERS purification tube, and carrying out high-speed centrifugation to obtain a supernatant;
s3, detecting the gas phase,
the gas chromatograph is a GC-6820 model of Agilent, USA, and an Electron Capture Detector (ECD), and the chromatographic column is a ZB-50 model with a specification of 30mx0.53mmx0.25 μm. Working conditions of the gas chromatograph: no split sample inlet, sample inlet temperature: 280 ℃; ECD detector temperature: 300 ℃; the column temperature procedure was: heating to 220 deg.C for 10min, and heating to 300 deg.C at 30 deg.C/min (maintaining for 15 min); carrier gas: is high-purity nitrogen, and the nitrogen purity is as follows: 99.999 percent; sample introduction amount: 1 mu L of the solution;
s4, detecting the recovery rate,
taking green vegetables as samples to perform recovery rate tests of 3 concentrations of dimethoate, omethoate, chlorpyrifos and phorate solution, repeating the tests for 3 times, and determining the accuracy and precision of the method; meanwhile, according to the pretreatment procedure of the method, 9 common pesticides such as cypermethrin and the like are selected, and when the addition concentration is 0.1mg/kg, the addition recovery rate test of hot pepper, quintozene, vinclozolin, chlorothalonil, triadimefon, dicofol, procymidone, bifenthrin and fenpropathrin is carried out, and the applicability of the method to the common pesticides is examined;
s5, analyzing the result,
selecting low, medium and high 3 concentrations in the linear range of the working curve, taking the signal-to-noise ratio of a chromatographic peak of the compound to be detected equal to 3 as the detection limit of the method, and taking the mass concentration corresponding to S/N (S/N) 10 as the quantification limit of the method.
The linear relation and the minimum detection concentration of 15 pesticides such as fluopicolide are as follows:
the test result of the addition recovery rate of the pesticide on the green vegetables is as follows:
the working principle of the invention is as follows:
gas chromatography refers to a column chromatography separation technique using a gas as a mobile phase. At present, the technology is widely applied to safety inspection and detection of health-care food, common food, water and the like. Among the 450 items tested and tested by the food, the test items of gas chromatography are already 125 items, the proportion is up to 28 percent, and the test items become an indispensable test technology in food safety test. The content of food safety detection by using the gas chromatography comprises the measurement of environmental pollutants and pesticide residues contained in food. For example, the residual quantity of trichlorfon, monocrotophos, phoxim, malathion, bifenthrin and the like in food is measured, and the residual quantity of organophosphorus pesticide in vegetables, fruits and the like is measured. Also included is the determination of the amount of additive present in the food product. Such as measuring the content of benzoic acid, sorbic acid, dehydroacetic acid, benzoyl peroxide, etc., present in the food product.
In conclusion, the method has the advantages of simplicity and convenience in operation, high sensitivity, good accuracy and the like. The method has the advantages of reducing the consumption of the solvent, saving time, being suitable for quickly screening the residual pesticides in the vegetable sample, having higher detection effectiveness and being worthy of popularization and application.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It should be understood by those skilled in the art that the foregoing embodiments are merely illustrative of the technical spirit and features of the present invention, and the present invention is not limited thereto but may be implemented by those skilled in the art.
Claims (3)
1. A method for measuring pesticide residue in vegetables by gas chromatography is characterized in that: the method comprises the following steps:
s1, pre-treating a sample,
fully crushing and uniformly mixing a vegetable sample by using a food processor to prepare a uniform sample to be detected, weighing 15.00g of the uniform sample to be detected in a 200mL flask, adding 15mL of acetonitrile, homogenizing for 90s by using a high-speed homogenizer, filtering into a measuring cylinder with a plug, fully shaking, and standing for 25min, wherein 5g of sodium chloride is placed in the measuring cylinder in advance; transferring 15mL of supernatant into a small beaker, adding about 8g of anhydrous sodium sulfate, and uniformly mixing;
s2, purifying the waste water,
adding the uniformly mixed solution into a centrifuge tube, carrying out vortex on a vortex mixer for 10min, centrifuging for 5min at 4000r/min, collecting acetonitrile solution to a concentration bottle, adding 5mL of acetonitrile for repeated extraction, combining extracting solutions, carrying out nitrogen blowing concentration to a constant volume of 5mL, accurately taking out 2mL of the acetonitrile solution, blowing the nitrogen to near dryness, carrying out acetone constant volume to 2mL, purifying by a QuEChERS purification tube, and carrying out high-speed centrifugation to obtain a supernatant;
s3, detecting the gas phase,
working conditions of the gas chromatograph: no split sample inlet, sample inlet temperature: 280 ℃; ECD detector temperature: 300 ℃; the column temperature procedure was: heating to 220 deg.C for 10min, and heating to 300 deg.C at 30 deg.C/min (maintaining for 15 min); carrier gas: is high-purity nitrogen; sample introduction amount: 1 mu L of the solution;
s4, detecting the recovery rate,
taking green vegetables as samples to perform recovery rate tests of 3 concentrations of dimethoate, omethoate, chlorpyrifos and phorate solution, repeating the tests for 3 times, and determining the accuracy and precision of the method; meanwhile, according to the pretreatment procedure of the method, 9 common pesticides such as cypermethrin and the like are selected, and when the addition concentration is 0.1mg/kg, the addition recovery rate test of hot pepper, quintozene, vinclozolin, chlorothalonil, triadimefon, dicofol, procymidone, bifenthrin and fenpropathrin is carried out, and the applicability of the method to the common pesticides is examined;
s5, analyzing the result,
selecting low, medium and high 3 concentrations in the linear range of the working curve, taking the signal-to-noise ratio of a chromatographic peak of the compound to be detected equal to 3 as the detection limit of the method, and taking the mass concentration corresponding to S/N (S/N) 10 as the quantification limit of the method.
2. The method for measuring pesticide residues in vegetables by using the gas chromatography as claimed in claim 1, wherein the method comprises the following steps: s3, a gas chromatograph for gas phase detection adopts a GC-6820 model of Agilent company in America, an Electron Capture Detector (ECD) is distributed, and a chromatographic column adopts a ZB-50 model with the specification of 30mx0.53mmx0.25 mu m.
3. The method for measuring pesticide residues in vegetables by using the gas chromatography as claimed in claim 1, wherein the method comprises the following steps: s3, nitrogen purity in gas phase detection: 99.999 percent.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103472155A (en) * | 2013-09-29 | 2013-12-25 | 邬金飞 | Gas chromatographic method for detecting residue amount of nine kinds of organophosphorus pesticide in rice |
| CN104678024A (en) * | 2015-03-12 | 2015-06-03 | 郭庆龙 | ECD determination method for residual quantity of N-(3-chloro-5-(trichloromethyl)pyridyl-2-methyl)-2,3,5,6-tetrafluoro-4-methoxybenzamide in vegetables and fruits |
| CN104713974A (en) * | 2015-04-10 | 2015-06-17 | 中国热带农业科学院农产品加工研究所 | Method for determining 55 kinds of pesticide residues in vegetable |
| CN105675742A (en) * | 2015-04-19 | 2016-06-15 | 盐城市农产品质量监督检验测试中心 | Quantitative detection and rapid pretreatment method of pesticide residues in fruits and vegetables |
-
2019
- 2019-11-26 CN CN201911174835.8A patent/CN110824060A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103472155A (en) * | 2013-09-29 | 2013-12-25 | 邬金飞 | Gas chromatographic method for detecting residue amount of nine kinds of organophosphorus pesticide in rice |
| CN104678024A (en) * | 2015-03-12 | 2015-06-03 | 郭庆龙 | ECD determination method for residual quantity of N-(3-chloro-5-(trichloromethyl)pyridyl-2-methyl)-2,3,5,6-tetrafluoro-4-methoxybenzamide in vegetables and fruits |
| CN104713974A (en) * | 2015-04-10 | 2015-06-17 | 中国热带农业科学院农产品加工研究所 | Method for determining 55 kinds of pesticide residues in vegetable |
| CN105675742A (en) * | 2015-04-19 | 2016-06-15 | 盐城市农产品质量监督检验测试中心 | Quantitative detection and rapid pretreatment method of pesticide residues in fruits and vegetables |
Non-Patent Citations (1)
| Title |
|---|
| 黎其万等: "蔬菜中31种农药残留量的气相色谱测定", 《云南农业大学学报》 * |
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