CN105548391A - Method for detecting residues of organochlorine and pyrethrin at different positions in vegetables - Google Patents
Method for detecting residues of organochlorine and pyrethrin at different positions in vegetables Download PDFInfo
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- CN105548391A CN105548391A CN201510920470.4A CN201510920470A CN105548391A CN 105548391 A CN105548391 A CN 105548391A CN 201510920470 A CN201510920470 A CN 201510920470A CN 105548391 A CN105548391 A CN 105548391A
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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
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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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
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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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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Abstract
The invention discloses a method for detecting residues of organochlorine and pyrethrin at different positions in vegetables, wherein the method includes the steps: (1) sampling: taking not less than 500 g of vegetable leaves and vegetable stems; (2) extracting: respectively weighing vegetable samples comprising 25 g of the vegetable leaves and 25 g of the vegetable stems; (3) suction filtration; (4) preparation of a chromatographic column; (5) purification and concentration; (6) production of a gas chromatographic reference; (7) recording of the chromatographic retention time and peak height of an extract liquid; and (8) establishment of a standard atlas and contrast analysis. By the way, the invention provides the method for detecting the residues of organochlorine and pyrethrin at different positions in the vegetables, the method respectively detects the contents of the drugs of organochlorine and pyrethrin of the vegetable stems and vegetable leaves of the vegetables, is convenient to detect and high in accuracy, can remind eaters the contents of the pesticide residue components at different positions in the vegetables, allows the eaters to select according to needs when eating the vegetables, and facilitates human body health.
Description
Technical field
The present invention relates to Detecting Pesticide, particularly relate to a kind of organochlorine, the pyrethrins detection method that diverse location is residual in vegetables.
Background technology
Organic chlorine agriculture chemicals, pyrethrins are class high-efficient broad-spectrum insecticides, are widely used in agriculture deinsectization by people.And organochlorine stable chemical nature, fat capacitive is large, and energy extended residual, in soil, air and water, has serious harm to health.And pyrethrins has great harm to human body and environment equally.
In the green advocated people, aseptic vegetables, green vegetables are non-existent completely.In order to not affect the healthy of people, must detect above-mentioned agricultural chemicals, guaranteeing the use safety of people.
Summary of the invention
The technical matters that the present invention mainly solves is to provide a kind of organochlorine, the pyrethrins detection method that diverse location is residual in vegetables, the organochlorine of vegetables Chinese food stem and dish leaf, chrysanthemum ester similar drug content are detected respectively, easy to detect, accuracy is high, can remind eater vegetables in diverse location residues of pesticides composition number, select as required time edible, be conducive to health.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: provide a kind of organochlorine, the pyrethrins detection method that diverse location is residual in vegetables, comprise the following steps: successively
(1) sample: get the vegetable leaf and vegetables stem that are no less than 500g, dish leaf and dish stem cutting knife are separated, air pressure is utilized to blow away the attachment on dish leaf and dish stem surface, dish leaf and dish stem are respectively charged in two different comminutors and pulverize, then be divided in different vials, keep sample for subsequent use;
(2) extract: take 25g dish leaf and 25g dish stem dish sample respectively, be placed in two different manual stamping machines, 35mL acetone and 35mL sherwood oil is added in dish leaf sampling stamping machine, 35mL acetone and 35mL sherwood oil is added equally in dish stem dish sample stamping machine, smash 3min clock respectively to pieces, then respectively the liquid in the liquid in dish leaf stamping machine and dish stem stamping machine is carried out suction filtration;
(3) extract: dish stem is smashed to pieces liquid and dish leaf smashs the aqueous sodium persulfate solution that liquid puts into two 150mL respectively to pieces, wherein, the content of sodium sulphate is 5g/100mL, evenly rock, static layering, then uses petroleum ether extraction, then utilizes in pipes type steaming valve device that to carry out evaporation and concentration for subsequent use;
(4) preparation of chromatographic column: add 3cm anhydrous sodium sulfate in glass chromatography column, then add 8 grams of water deactivation florisil silicas, adding 2cm anhydrous sodium sulfate, make decontaminating column;
(5) purification is with concentrated: draw 10mL dish leaf extract and dish stem extract respectively, add different decontaminating columns, be then settled to 5mL;
(6) gas chromatography reference is made: be 0.35mm by internal diameter, the quartz elastic capillary tube post of long 10mm is put into heating cabinet and is heated up, the temperature of quartzy tubing string is made to be 180 ~ 250 DEG C, then at insulation 5min, the dish leaf extract of 5mL, dish stem extract are put into different quartz ampoule tubing strings respectively, record chromatographic retention and peak height; Criterion collection of illustrative plates is 0.01mg/L, 0.05mg/L with thinning agent compound concentration, the organochlorine of 0.1mg/L, 0.5mg/L, 1.0mg/L, pyrethrins standard solution, then put into quartzy tubing string with series standard solution to detect, record chromatographic retention and peak height, be analyzed.
In the present invention's preferred embodiments, when described step (3) PetroChina Company Limited. ether extraction dish leaf extract, dish footpath extract, through 4 extractions, extract 2.5mL at every turn.
In the present invention's preferred embodiments, in described step (4), decontaminating column is interior through sherwood oil drip washing, and cylinder leaves 0.5 ~ 0.9mL liquid.
In the present invention's preferred embodiments, in described step (6), thinning agent is normal hexane.
The invention has the beneficial effects as follows: a kind of organochlorine of the present invention, the pyrethrins detection method that diverse location is residual in vegetables, vegetables Chinese food footpath and the organochlorine of dish leaf, the content of pyrethrins are detected respectively, easy to detect, accuracy is high, can remind eater vegetables in diverse location residues of pesticides composition number, select as required time edible, be conducive to health.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making other embodiments all obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
Organochlorine, the pyrethrins detection method that diverse location is residual in vegetables, is characterized in that, comprise the following steps: successively
(1) sample: get the vegetable leaf and vegetables stem that are no less than 500g, dish leaf and dish stem cutting knife are separated, air pressure is utilized to blow away the attachment on dish leaf and dish stem surface, dish leaf and dish stem are respectively charged in two different comminutors and pulverize, then be divided in different vials, keep sample for subsequent use;
(2) extract: take 25g dish leaf and 25g dish stem dish sample respectively, be placed in two different manual stamping machines, 35mL acetone and 35mL sherwood oil is added in dish leaf sampling stamping machine, 35mL acetone and 35mL sherwood oil is added equally in dish stem dish sample stamping machine, smash 3min clock respectively to pieces, then respectively the liquid in the liquid in dish leaf stamping machine and dish stem stamping machine is carried out suction filtration;
(3) extract: dish stem is smashed to pieces liquid and dish leaf smashs the aqueous sodium persulfate solution that liquid puts into two 150mL respectively to pieces, wherein, the content of sodium sulphate is 5g/100mL, evenly rock, static layering, then with sherwood oil through 4 extractions, extract 2.5mL, it is for subsequent use to carry out evaporation and concentration in recycling pipes type steaming valve device at every turn;
(4) preparation of chromatographic column: add 3cm anhydrous sodium sulfate in glass chromatography column, then add 8 grams of water deactivation florisil silicas, adding 2cm anhydrous sodium sulfate, make decontaminating column;
(5) purification is with concentrated: draw 10mL dish leaf extract and dish stem extract respectively, add different decontaminating columns, be then settled to 5mL;
(6) make gas chromatography reference: be 0.35mm by internal diameter, the quartz elastic capillary tube post of long 10mm is put into heating cabinet and is heated up, and makes the temperature of quartzy tubing string be 250 DEG C, then at insulation 5min; The dish leaf extract of 5mL, dish stem extract are put into different quartz ampoule tubing strings respectively, record chromatographic retention and peak height; Criterion collection of illustrative plates, is organochlorine, the pyrethrins standard solution of 0.01mg/L with normal hexane compound concentration, then puts into quartzy tubing string with series standard solution and detect, and record chromatographic retention and peak height, be analyzed.
In described step (4), decontaminating column is interior through sherwood oil drip washing, and cylinder leaves 0.9mL liquid.
Embodiment 2
Organochlorine, the pyrethrins detection method that diverse location is residual in vegetables, is characterized in that, comprise the following steps: successively
(1) sample: get the vegetable leaf and vegetables stem that are no less than 400g, dish leaf and dish stem cutting knife are separated, air pressure is utilized to blow away the attachment on dish leaf and dish stem surface, dish leaf and dish stem are respectively charged in two different comminutors and pulverize, then be divided in different vials, keep sample for subsequent use;
(2) extract: take 25g dish leaf and 25g dish stem dish sample respectively, be placed in two different manual stamping machines, 35mL acetone and 35mL sherwood oil is added in dish leaf sampling stamping machine, 35mL acetone and 35mL sherwood oil is added equally in dish stem dish sample stamping machine, smash 3min clock respectively to pieces, then respectively the liquid in the liquid in dish leaf stamping machine and dish stem stamping machine is carried out suction filtration;
(3) extract: dish stem is smashed to pieces liquid and dish leaf smashs the aqueous sodium persulfate solution that liquid puts into two 150mL respectively to pieces, wherein, the content of sodium sulphate is 5g/100mL, evenly rock, static layering, then with sherwood oil through 4 extractions, extract 2.5mL, it is for subsequent use to carry out evaporation and concentration in recycling pipes type steaming valve device at every turn;
(4) preparation of chromatographic column: add 3cm anhydrous sodium sulfate in glass chromatography column, then add 8 grams of water deactivation florisil silicas, adding 2cm anhydrous sodium sulfate, make decontaminating column;
(5) purification is with concentrated: draw 10mL dish leaf extract and dish stem extract respectively, add different decontaminating columns, be then settled to 5mL;
(6) make gas chromatography reference: be 0.35mm by internal diameter, the quartz elastic capillary tube post of long 10mm is put into heating cabinet and is heated up, and makes the temperature of quartzy tubing string be 180 DEG C, then at insulation 5min; The dish leaf extract of 5mL, dish stem extract are put into different quartz ampoule tubing strings respectively, record chromatographic retention and peak height; Criterion collection of illustrative plates, is organochlorine, the pyrethrins standard solution of 1.0mg/L with normal hexane compound concentration, then puts into quartzy tubing string with series standard solution and detect, and record chromatographic retention and peak height, be analyzed.
In described step (4), decontaminating column is interior through sherwood oil drip washing, and cylinder leaves 0.6mL liquid.
The beneficial effect of the invention is: a kind of organochlorine of the present invention, the pyrethrins detection method that diverse location is residual in vegetables, the organochlorine of vegetables Chinese food stem and dish leaf, chrysanthemum ester similar drug content are detected respectively, easy to detect, accuracy is high, the residues of pesticides composition of diverse location in can reminding eater vegetables.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize instructions of the present invention to do equivalent structure or the conversion of equivalent flow process, or be directly or indirectly used in other relevant technical field, be all in like manner included in scope of patent protection of the present invention.
Claims (4)
1. organochlorine, the pyrethrins detection method that diverse location is residual in vegetables, is characterized in that, comprise the following steps: successively
(1) sample: get the vegetable leaf and vegetables stem that are no less than 500g, dish leaf and dish stem cutting knife are separated, air pressure is utilized to blow away the attachment on dish leaf and dish stem surface, dish leaf and dish stem are respectively charged in two different comminutors and pulverize, then be divided in different vials, keep sample for subsequent use;
(2) extract: take 25g dish leaf and 25g dish stem dish sample respectively, be placed in two different manual stamping machines, 35mL acetone and 35mL sherwood oil is added in dish leaf sampling stamping machine, 35mL acetone and 35mL sherwood oil is added equally in dish stem dish sample stamping machine, smash 3min clock respectively to pieces, then respectively the liquid in the liquid in dish leaf stamping machine and dish stem stamping machine is carried out suction filtration;
(3) extract: dish stem is smashed to pieces liquid and dish leaf smashs the aqueous sodium persulfate solution that liquid puts into two 150mL respectively to pieces, wherein, the content of sodium sulphate is 5g/100mL, evenly rock, static layering, then uses petroleum ether extraction, and it is for subsequent use to carry out evaporation and concentration in recycling pipes type steaming valve device;
(4) preparation of chromatographic column: add 3cm anhydrous sodium sulfate in glass chromatography column, then add 8 grams of water deactivation florisil silicas, adding 2cm anhydrous sodium sulfate, make decontaminating column;
(5) purification is with concentrated: draw 10mL dish leaf extract and dish stem extract respectively, add different decontaminating columns, be then settled to 5mL;
(6) make gas chromatography reference: be 0.35mm by internal diameter, the quartz elastic capillary tube post of long 10mm is put into heating cabinet and is heated up, and makes the temperature of quartzy tubing string be 180 ~ 250 DEG C, then at insulation 5min; The dish leaf extract of 5mL, dish stem extract are put into different quartz ampoule tubing strings respectively, record chromatographic retention and peak height; Criterion collection of illustrative plates is 0.01mg/L, 0.05mg/L with thinning agent compound concentration, the organochlorine of 0.1mg/L, 0.5mg/L, 1.0mg/L, pyrethrins standard solution, then put into quartzy tubing string with series standard solution to detect, record chromatographic retention and peak height, be analyzed.
2. organochlorine according to claim 1, the pyrethrins detection method that diverse location is residual in vegetables, it is characterized in that, when described step (3) PetroChina Company Limited. ether extraction dish leaf extract, dish stem extract, through 4 extractions, extract 2.5mL at every turn.
3. organochlorine according to claim 1, the pyrethrins detection method that diverse location is residual in vegetables, in described step (4), decontaminating column is interior through sherwood oil drip washing, and cylinder leaves 0.5 ~ 0.9mL liquid.
4. organochlorine according to claim 1, the pyrethrins detection method that diverse location is residual in vegetables, in described step (6), thinning agent is normal hexane.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510920470.4A CN105548391A (en) | 2015-12-11 | 2015-12-11 | Method for detecting residues of organochlorine and pyrethrin at different positions in vegetables |
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| CN201510920470.4A CN105548391A (en) | 2015-12-11 | 2015-12-11 | Method for detecting residues of organochlorine and pyrethrin at different positions in vegetables |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106645465A (en) * | 2016-11-29 | 2017-05-10 | 保山市质量技术监督综合检测中心 | Method for determining organochlorine and pyrethroid pesticide residues in fresh Dendrobium strips |
| CN109270033A (en) * | 2018-09-10 | 2019-01-25 | 南京市产品质量监督检验院 | The rapid detection method of Hazard factor in a kind of food |
| CN109856230A (en) * | 2019-01-30 | 2019-06-07 | 山东博戎伝创信息科技有限公司 | Organic compound residue analysis method and device and intelligent monitoring system thereof |
-
2015
- 2015-12-11 CN CN201510920470.4A patent/CN105548391A/en active Pending
Non-Patent Citations (4)
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| 中华人民共和国卫生部中国国家标准化管理委员会: "《中华人民共和国国家标准GB/T 5009.146-2008》", 1 March 2009 * |
| 杨淑娟 等: "蔬菜中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类33种农药多残留测定", 《漳州职业技术学院学报》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106645465A (en) * | 2016-11-29 | 2017-05-10 | 保山市质量技术监督综合检测中心 | Method for determining organochlorine and pyrethroid pesticide residues in fresh Dendrobium strips |
| CN109270033A (en) * | 2018-09-10 | 2019-01-25 | 南京市产品质量监督检验院 | The rapid detection method of Hazard factor in a kind of food |
| CN109856230A (en) * | 2019-01-30 | 2019-06-07 | 山东博戎伝创信息科技有限公司 | Organic compound residue analysis method and device and intelligent monitoring system thereof |
| CN109856230B (en) * | 2019-01-30 | 2021-09-21 | 山东博戎伝创信息科技有限公司 | Organic compound residue analysis method and device and intelligent monitoring system thereof |
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Application publication date: 20160504 |