CN106018048A - Pretreatment method for detection of multiple pesticide residues in fruit and vegetable samples - Google Patents
Pretreatment method for detection of multiple pesticide residues in fruit and vegetable samples Download PDFInfo
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- CN106018048A CN106018048A CN201610330981.5A CN201610330981A CN106018048A CN 106018048 A CN106018048 A CN 106018048A CN 201610330981 A CN201610330981 A CN 201610330981A CN 106018048 A CN106018048 A CN 106018048A
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- acetonitrile
- sample
- fruit
- toluene
- volume ratio
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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
- G01N1/34—Purifying; Cleaning
Abstract
The invention discloses a pretreatment method for detection of multiple pesticide residues in fruit and vegetable samples. The pretreatment method comprises steps as follows: the samples are sampled with a quartation method and produced in a form of mud, and the mud-like samples are put in a centrifuge tube; acetonitrile is added to the centrifuge tube, homogenization is performed, sodium chloride is added, centrifugation is performed again after homogenization, a centrifuged supernatant is taken, put in a heart-shaped specimen bottle and subjected to rotary evaporation until the supernatant is almost dry, a mixed liquid of acetonitrile and toluene in the volume ratio being 3:1 is added and subjected to ultrasonic dissolution, and an extracting solution is obtained; after anhydrous sodium sulfate is added to a chromatographic column, activation is performed by means of the mixed liquid of acetonitrile and toluene in the volume ratio being 3:1, the extracting solution is added, leaching is performed by means of the mixed liquid of acetonitrile and toluene in the volume ratio being 3:1, a leaching liquid is collected and put in the heart-shaped specimen bottle for standby use, the leaching liquid in the heart-shaped specimen bottle is subjected to rotary evaporation until the leaching liquid is almost dry, acetone is added for ultrasonic dissolution, and a product is bottled and checked on a machine. The method is simple, sensitive, rapid, accurate and suitable for confirmation analysis of various pesticide residues.
Description
Technical field
The present invention relates to the Detection Technologies of Pesticide Residues field, particularly to multi-pesticide residue residual in a kind of fruit and vegerable sample
The pre-treating method of detection.
Background technology
At present, the important measures of prevention and elimination of disease and pests during chemical prevention is agricultural production.Pesticide use in a large number and
Method of application is unreasonable causes pesticide residue in agricultural products to rise.Pesticide Residue becomes affects agricultural product
The major issue of quality safety.Improve constantly along with living standards of the people and to healthy attention degree, food
Product safety problem is increasingly becoming people's focus of attention.Agricultural product for preventing pesticide residues from exceeding standard come into the market,
Aobvious particularly important for Residual Pesticides in Farm Produce detection.
The detection of Residual Pesticides in Farm Produce mainly includes Sample Pretreatment Technique and analysis and detection technology.Sample
Pre-treatment is the committed step analyzing detection, directly determines correctness and the objectivity of analysis result.Meanwhile,
Time needed for analyzing the pre-treatment of sample accounts for whole analysis process more than 60%.Sample pre-treatments relates to step
The most various, mainly include the preparation of sample, extracting and developing, purification etc., whole flow process wastes time and energy, effect
Rate is low.At present, in fruit and vegerable, the detection method of multi-pesticide residue has a lot, most GB/T19648-2006 that use, but
The pretreatment process of this kind of detection method has the following disadvantages:
1. purification is made is not very abundant, especially for the sample that pigment content is more；
2. the clean-up effect for allium vegetables is bad, and the interference on FPD can be bigger；
3. pre-treatment operating procedure is complicated, and the amount of reagent of consumption is big, and sample processing time is long, when for high-volume
During the detection of sample inefficient.
Summary of the invention
The invention provides the pre-treating method of multi-pesticide residue residue detection in a kind of fruit and vegerable sample, solve existing
The problem that in pretreatment process, clean-up effect is bad and pre-treatment operating procedure is complicated.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
The pre-treating method of multi-pesticide residue residue detection in a kind of fruit and vegerable sample, comprises the following steps:
(1) prefabricated: by sample according to sample quarterlies after, make pureed, be placed in centrifuge tube；
(2) extract: centrifuge tube adds acetonitrile, homogenate, add sodium chloride, again centrifugal after homogenate, take
Supernatant after Li Xin is in Cor Gigeriae Galli bottle, and rotary evaporation is the most dry, adds volume ratio and is the acetonitrile of 3:1 and toluene mixes
Close liquid, ultrasonic dissolution, obtain extracting solution；
(3) purify: after chromatographic column adds anhydrous sodium sulfate, mix with the acetonitrile that volume ratio is 3:1 and toluene
Close liquid to activate, add extracting solution, carry out drip washing with the acetonitrile that volume ratio is 3:1 and toluene mixture liquid, receive
Collect leacheate standby in Cor Gigeriae Galli bottle, by the most dry for the leacheate rotary evaporation in Cor Gigeriae Galli bottle, add acetone solution
After ultrasonic, machine testing in bottling.
Wherein it is preferred to, in described step (2), the temperature of rotary evaporation is 30～50 DEG C.
Wherein it is preferred to, in described step (3), the temperature of rotary evaporation is 30～50 DEG C.
Wherein it is preferred to, described chromatographic column is Carb-NH2 post, adds anhydrous in described Carb-NH2 post
The height of sodium sulfate is 2cm.
Beneficial effects of the present invention:
Good purification the most of the present invention, it is possible to effectively remove pigment in sample；
Pre-treatment operating procedure the most of the present invention is simple, original twin columns purify and be simplified to single-column purification；
3. the method choice of the present invention is good, and capacity of resisting disturbance is strong, and the method after improvement can be good at removing sample
Impurity in product substrate, is effectively kept target compound；
4. the inventive method is simple, sensitive, quick, accurate, is suitable for the confirmatory analysis of Multi-pesticide residues.
Detailed description of the invention
Below technical scheme is clearly and completely described, it is clear that described content is only
It is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, this
The every other embodiment that field those of ordinary skill is obtained under not making creative work premise, all
Belong to the scope of protection of the invention.
The pre-treating method of multi-pesticide residue residue detection in a kind of fruit and vegerable sample, comprises the following steps:
(1) prefabricated: by sample according to sample quarterlies after, make pureed, be placed in centrifuge tube；
(2) extract: centrifuge tube adds acetonitrile, homogenate, add sodium chloride, again centrifugal after homogenate, take
Supernatant after Li Xin is in Cor Gigeriae Galli bottle, and rotary evaporation is the most dry, adds volume ratio and is the acetonitrile of 3:1 and toluene mixes
Close liquid, ultrasonic dissolution, obtain extracting solution；
(3) purify: after chromatographic column adds anhydrous sodium sulfate, mix with the acetonitrile that volume ratio is 3:1 and toluene
Close liquid to activate, add extracting solution, carry out drip washing with the acetonitrile that volume ratio is 3:1 and toluene mixture liquid, receive
Collect leacheate standby in Cor Gigeriae Galli bottle, by the most dry for the leacheate rotary evaporation in Cor Gigeriae Galli bottle, add acetone solution
After ultrasonic, machine testing in bottling.
Embodiment 1
The present embodiment provides the pre-treating method of multi-pesticide residue residue detection in a kind of fruit and vegerable sample, including following step
Rapid:
(1) prefabricated: by sample according to sample quarterlies after, make pureed, accurately strive for that 20.0g is in 80ml
In centrifuge tube；
(2) extract: centrifuge tube adds 40ml acetonitrile, after homogenate 1min, add 5.0g sodium chloride, then
It is centrifuged after secondary homogenate 1min；Take centrifugal after supernatant 20ml in Cor Gigeriae Galli bottle, 40 DEG C of rotary evaporations are the most dry,
Add 4ml acetonitrile/toluene (3:1), ultrasonic dissolution.
(3) purify: after chromatographic column (Carb-NH2) adds 2cm anhydrous sodium sulfate, use 10ml acetonitrile
/ toluene (3:1) activates, and adds 4ml extracting solution, carries out drip washing with 16ml acetonitrile/toluene (3:1),
Collect leacheate standby in Cor Gigeriae Galli bottle.Leacheate in Cor Gigeriae Galli bottle is the most dry in 40 DEG C of rotary evaporations, add
After 4ml acetone solution is ultrasonic, machine testing in bottling.
Embodiment 2
The present embodiment provides the pre-treating method of multi-pesticide residue residue detection in a kind of fruit and vegerable sample, including following step
Rapid:
(1) prefabricated: by sample according to sample quarterlies after, make pureed, accurately strive for that 20.0g is in 80ml
In centrifuge tube；
(2) extract: centrifuge tube adds 40ml acetonitrile, after homogenate 1min, add 5.0g sodium chloride, then
It is centrifuged after secondary homogenate 1min；Take centrifugal after supernatant 20ml in Cor Gigeriae Galli bottle, 30 DEG C of rotary evaporations are the most dry,
Add 4ml acetonitrile/toluene (3:1), ultrasonic dissolution.
(3) purify: after chromatographic column (Carb-NH2) adds 2cm anhydrous sodium sulfate, use 10ml acetonitrile
/ toluene (3:1) activates, and adds 4ml extracting solution, carries out drip washing with 16ml acetonitrile/toluene (3:1),
Collect leacheate standby in Cor Gigeriae Galli bottle.Leacheate in Cor Gigeriae Galli bottle is the most dry in 50 DEG C of rotary evaporations, add
After 4ml acetone solution is ultrasonic, machine testing in bottling.
Embodiment 3
The present embodiment provides the pre-treating method of multi-pesticide residue residue detection in a kind of fruit and vegerable sample, including following step
Rapid:
(1) prefabricated: by sample according to sample quarterlies after, make pureed, accurately strive for that 20.0g is in 80ml
In centrifuge tube；
(2) extract: centrifuge tube adds 40ml acetonitrile, after homogenate 1min, add 5.0g sodium chloride, then
It is centrifuged after secondary homogenate 1min；Take centrifugal after supernatant 20ml in Cor Gigeriae Galli bottle, 30 DEG C of rotary evaporations are the most dry,
Add 4ml acetonitrile/toluene (3:1), ultrasonic dissolution.
(3) purify: after chromatographic column (Carb-NH2) adds 2cm anhydrous sodium sulfate, use 10ml acetonitrile
/ toluene (3:1) activates, and adds 4ml extracting solution, carries out drip washing with 16ml acetonitrile/toluene (3:1),
Collect leacheate standby in Cor Gigeriae Galli bottle.Leacheate in Cor Gigeriae Galli bottle is the most dry in 50 DEG C of rotary evaporations, add
After 4ml acetone solution is ultrasonic, machine testing in bottling.
Application examples 1
The pre-treating method using the present invention does recovery test, with the pre-treatment using GB/T19648-2006
Method contrasts, and result of the test is as follows:
From upper watch test data, the pre-treating method response rate of the present invention be apparently higher than
The method of GB/T19648-2006.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all at this
Within bright spirit and principle, any modification, equivalent substitution and improvement etc. made, should be included in this
Within bright protection domain.
Claims (4)
1. the pre-treating method of multi-pesticide residue residue detection in a fruit and vegerable sample, it is characterised in that include following step
Rapid:
(1) prefabricated: by sample according to sample quarterlies after, make pureed, be placed in centrifuge tube；
(2) extract: centrifuge tube adds acetonitrile, homogenate, add sodium chloride, again centrifugal after homogenate, take
Supernatant after Li Xin is in Cor Gigeriae Galli bottle, and rotary evaporation is the most dry, adds volume ratio and is the acetonitrile of 3:1 and toluene mixes
Close liquid, ultrasonic dissolution, obtain extracting solution；
(3) purify: after chromatographic column adds anhydrous sodium sulfate, mix with the acetonitrile that volume ratio is 3:1 and toluene
Close liquid to activate, add extracting solution, carry out drip washing with the acetonitrile that volume ratio is 3:1 and toluene mixture liquid, receive
Collect leacheate standby in Cor Gigeriae Galli bottle, by the most dry for the leacheate rotary evaporation in Cor Gigeriae Galli bottle, add acetone solution
After ultrasonic, machine testing in bottling.
In a kind of fruit and vegerable sample the most according to claim 1 in fruit and vegerable sample before multi-pesticide residue residue detection
Processing method, it is characterised in that in described step (2), the temperature of rotary evaporation is 30～50 DEG C.
The front place of multi-pesticide residue residue detection in fruit and vegerable sample in a kind of vegetables sample the most according to claim 1
Reason method, it is characterised in that in described step (3), the temperature of rotary evaporation is 30～50 DEG C.
The front place of multi-pesticide residue residue detection in fruit and vegerable sample in a kind of vegetables sample the most according to claim 1
Reason method, it is characterised in that described chromatographic column is Carb-NH2 post, adds nothing in described Carb-NH2 post
The height of aqueous sodium persulfate is 2cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610330981.5A CN106018048A (en) | 2016-05-18 | 2016-05-18 | Pretreatment method for detection of multiple pesticide residues in fruit and vegetable samples |
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| CN201610330981.5A CN106018048A (en) | 2016-05-18 | 2016-05-18 | Pretreatment method for detection of multiple pesticide residues in fruit and vegetable samples |
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| CN201610330981.5A Pending CN106018048A (en) | 2016-05-18 | 2016-05-18 | Pretreatment method for detection of multiple pesticide residues in fruit and vegetable samples |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106644666A (en) * | 2017-02-10 | 2017-05-10 | 西南大学 | Method for removing pigment by pretreatment in agricultural residue detection of fruit and vegetable samples |
| CN107389808A (en) * | 2017-06-28 | 2017-11-24 | 防城港市质量技术监督局 | The detection method of vegetable pesticide residue |
| CN112083116A (en) * | 2020-09-29 | 2020-12-15 | 合肥海关技术中心 | Method for measuring residual quantity of prothioconazole and metabolite thioneazole thereof in apples |
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| CN102221589A (en) * | 2011-03-28 | 2011-10-19 | 中国水稻研究所 | Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer |
| CN102539578A (en) * | 2010-12-30 | 2012-07-04 | 宋国新 | Method for extracting pesticide residue of fragrant-flowered garlic |
| CN102600811A (en) * | 2012-03-31 | 2012-07-25 | 天津博纳艾杰尔科技有限公司 | Sample pretreatment method for tea leaf pesticide residue detection and tea leaf purification column |
| CN102735778A (en) * | 2012-07-09 | 2012-10-17 | 吴桂玲 | Pretreatment method for detecting organochlorine pesticide residue |
| CN103196886A (en) * | 2013-03-20 | 2013-07-10 | 厦门大学 | Detection method of organophosphorus pesticide residues in tea |
| CN103529153A (en) * | 2013-07-26 | 2014-01-22 | 宁波检验检疫科学技术研究院 | Common rapid detection method for various pesticide residues in soybeans |
| CN104764832A (en) * | 2015-04-29 | 2015-07-08 | 四川省农业科学院分析测试中心 | Detecting method of pesticide multi-residue in fresh tea leaves |
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2016
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539578A (en) * | 2010-12-30 | 2012-07-04 | 宋国新 | Method for extracting pesticide residue of fragrant-flowered garlic |
| CN102221589A (en) * | 2011-03-28 | 2011-10-19 | 中国水稻研究所 | Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer |
| CN102600811A (en) * | 2012-03-31 | 2012-07-25 | 天津博纳艾杰尔科技有限公司 | Sample pretreatment method for tea leaf pesticide residue detection and tea leaf purification column |
| CN102735778A (en) * | 2012-07-09 | 2012-10-17 | 吴桂玲 | Pretreatment method for detecting organochlorine pesticide residue |
| CN103196886A (en) * | 2013-03-20 | 2013-07-10 | 厦门大学 | Detection method of organophosphorus pesticide residues in tea |
| CN103529153A (en) * | 2013-07-26 | 2014-01-22 | 宁波检验检疫科学技术研究院 | Common rapid detection method for various pesticide residues in soybeans |
| CN104764832A (en) * | 2015-04-29 | 2015-07-08 | 四川省农业科学院分析测试中心 | Detecting method of pesticide multi-residue in fresh tea leaves |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106644666A (en) * | 2017-02-10 | 2017-05-10 | 西南大学 | Method for removing pigment by pretreatment in agricultural residue detection of fruit and vegetable samples |
| CN107389808A (en) * | 2017-06-28 | 2017-11-24 | 防城港市质量技术监督局 | The detection method of vegetable pesticide residue |
| CN112083116A (en) * | 2020-09-29 | 2020-12-15 | 合肥海关技术中心 | Method for measuring residual quantity of prothioconazole and metabolite thioneazole thereof in apples |
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Application publication date: 20161012 |