CN201903472U - Pretreatment reagent kit for dinitroaniline herbicide residues in fruit and vegetables - Google Patents
Pretreatment reagent kit for dinitroaniline herbicide residues in fruit and vegetables Download PDFInfo
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- CN201903472U CN201903472U CN2010206387689U CN201020638768U CN201903472U CN 201903472 U CN201903472 U CN 201903472U CN 2010206387689 U CN2010206387689 U CN 2010206387689U CN 201020638768 U CN201020638768 U CN 201020638768U CN 201903472 U CN201903472 U CN 201903472U
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- centrifuge tube
- dinitroaniline herbicide
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Abstract
The utility model relates to a pretreatment reagent kit for dinitroaniline herbicide residues in fruit and vegetables, which belongs to the technical field of food safety. The pretreatment reagent kit for the dinitroaniline herbicide residues in the fruit and the vegetables is characterized in that the pretreatment reagent kit comprises an extractant centrifuge tube, a dispersing agent centrifuge tube, a cleansing agent centrifuge tube and a needle tube filter. The extractant centrifuge tube, the dispersing agent centrifuge tube and the cleansing agent centrifuge tube are polypropylene centrifuge tubes with spiral covers, and the needle tube filter is composed of a cylindrical plug and a polyethylene cylinder. A lower stopping sieve plate, fillings and an upper stopping sieve plate are mounted inside the polyethylene cylinder from bottom to top. The pretreatment reagent kit for the dinitroaniline herbicide residues in the fruit and the vegetables is simple in structure, little in use of solvent, low in pollution to environment, fine in purifying effect, simple in operation, economical and practical, low in manufacturing cost, reliable in performance, wide in application range, and favorable for health of operators and the like.
Description
Technical field
The utility model belongs to the food security technical field, particularly relates to the residual pretreatment reagent kit of dinitroaniline herbicide in a kind of fruits and vegetables.
Background technology
At present, dinitroaniline (dinitroaniline) class herbicide is a kind of important selectivity preemergence herbicide, is widely used in crops such as vegetables such as cabbage, carrot, apple and fruit, and general structure is 2, the 6-dinitroaniline.Because such herbicide broad weed-killing spectrum, herbicidal effect are stablized, and have worldwide obtained widespread use.Because soil has strong suction-operated to paradinitrobenzene amine herbicide, its residual meeting produces poisoning to succession crop, and in the lymphocytic Using Comet Assay of the mankind, trefanocide has genotoxicity to mammalian cell.
But dinitroaniline herbicide detects relatively difficulty, detects individual event agricultural chemicals such as Pendimethalin or trefanocide, and operating process is loaded down with trivial details, and testing cost is high.Because the dinitroaniline herbicide residual quantity is lower in the fruits and vegetables matrix, serious interference and difficult the removal, literature search shows, fails to retrieve many method for detecting residue of dinitroaniline herbicide in the fruits and vegetables class matrix.
In the mensuration about single class medicine residues of pesticides such as Pendimethalins in the fruits and vegetables class sample of having reported, adopt traditional liquid-liquid extraction (LLE) method to extract object in the sample mostly.The a large amount of poisonous and hazardous organic solvents of this method consumption, loaded down with trivial details time-consuming, and in extraction process, be easy to generate a large amount of emulsions, influence extraction efficiency; So detect a kind of pretreatment technology device rapidly and efficiently of such material demand.
Summary of the invention
The utility model provides the residual pretreatment reagent kit of dinitroaniline herbicide in a kind of fruits and vegetables for solving the problem that prior art exists.
The utility model purpose provides a kind of extraction efficiency height and can effectively remove the how residual quick pretreatment reagent kit of dinitroaniline herbicide of impurity, it is residual to be used for quick pretreatment fruits and vegetables class sample dinitroaniline herbicide, and fruits and vegetables class sample can directly detect with analytical instrument after this kit is handled.The residual pretreatment reagent kit of dinitroaniline herbicide has simple in structurely in the fruits and vegetables, uses solvent few, low in the pollution of the environment, good purification, simple to operate, economical and practical, low cost of manufacture, dependable performance, applied range helps characteristics such as operating personnel are healthy.
The residual pretreatment reagent kit of dinitroaniline herbicide adopts following technical scheme in the utility model fruits and vegetables:
The residual pretreatment reagent kit of dinitroaniline herbicide in a kind of fruits and vegetables, be characterized in: kit comprises extraction agent, spreading agent, cleanser centrifuge tube and needle tube type filtrator, extraction agent, spreading agent, cleanser centrifuge tube are tool plug screw top polypropylene centrifuge tube, the needle tube type filtrator is made of column piston, tygon cylinder, retaining sieve plate, filler is housed down in the tygon cylinder from the bottom to top and goes up the retaining sieve plate.
The residual pretreatment reagent kit of dinitroaniline herbicide can also adopt following technical measures in the utility model fruits and vegetables:
The residual pretreatment reagent kit of dinitroaniline herbicide in the described fruits and vegetables is characterized in: the capacity that the extraction agent centrifuge tube is housed is 40-60mL, spreading agent is housed and cleanser centrifuge tube capacity is 15-20mL.
The residual pretreatment reagent kit of dinitroaniline herbicide in the described fruits and vegetables is characterized in: on keep off sieve plate and down the screen size of retaining sieve plate be 0.15-0.3 μ m.
The residual pretreatment reagent kit of dinitroaniline herbicide in the described fruits and vegetables is characterized in: filler is that florisil silica, C18 or Graphon purify filler.
The residual pretreatment reagent kit of dinitroaniline herbicide in the described fruits and vegetables is characterized in: extraction agent is acid chromatographically pure chemistry reagent.
The residual pretreatment reagent kit of dinitroaniline herbicide in the described fruits and vegetables is characterized in: spreading agent and cleanser are white particle or mixture of powders.
Advantage that the utlity model has and good effect:
The residual pretreatment reagent kit of dinitroaniline herbicide in the fruits and vegetables, owing to adopted the utility model brand-new technology scheme, compared with prior art, the utility model is based on the high selectivity extractability of extraction agent and spreading agent paradinitrobenzene amine herbicide and the cleanser effective removing ability to fruits and vegetables class sample impurity, realize efficiently, dinitroaniline matter selective separation in the fruits and vegetables class sample, purifying and enrichment fast, thereby make the subsequent detection method reach highly sensitive and the strong purpose of selectivity.The utility model is mainly used in the sample pre-treatments of dinitroaniline herbicide in the fruits and vegetables class sample, has the following advantages:
(1) simple, pollution-free, the room temperature preservation of production run, single part of mensuration; (2) operating process is simple, quick, and spent low, the pre-treatment process only needed about 20 minutes, and this point is applicable to the quick pretreatment of dinitroaniline herbicide class material; (3) extraction agent is through the saturated acetonitrile solution of normal hexane in the kit, reduced the extraction polarity of solvent, reduced the liquid water content in the moisture class matrix extract, alleviated the follow-up water pressure of removing, can target compound have been played a protective role and add 0.5% glacial acetic acid; Anhydrous magnesium sulfate also heat production in suction has promoted the extraction of target compound in the spreading agent, and disposable needle tube type filtrator can be removed many polarity matrix components as fatty acid, some polarity lipophilicity pigment and carbohydrate etc. from sample coextraction thing.
Description of drawings
Fig. 1 is the residual pretreatment reagent kit structural representation of dinitroaniline herbicide in the utility model fruits and vegetables;
Fig. 2 is common fruits and vegetables class sample with disposable needle tube type filtrator;
Fig. 3 is complex samples such as onion, garlic with disposable needle tube type filtrator.
Disposable needle tube type filtrator is provided with sieve plate, florisil silica layer, sieve plate, C18 or the Graphon layer of 0.22 μ m and the sieve plate of 0.22 μ m of 0.22 μ m from top to bottom successively.
Among the figure, 1, extraction agent, 2, spreading agent, 3, cleanser, 4, disposable needle tubing filtrator, 5, disposable needle tubing filtrator.
Embodiment
For further understanding technology contents of the present utility model, characteristics and effect, enumerate following example now, and conjunction with figs. is described in detail as follows:
With reference to accompanying drawing 1 to Fig. 3.
Embodiment 1
The how residual quick pretreatment reagent kit of dinitroaniline herbicide in the fruits and vegetables is made up of extraction agent 1, spreading agent 2, cleanser 3, one-shot injector formula filtration unit 4.Wherein, extraction agent is contained in the 50mL tool plug screw top polypropylene centrifuge tube, and spreading agent and cleanser are contained in the 15mL tool plug screw top polypropylene centrifuge tube.Wherein disposable needle tubing filtration unit is made of retaining sieve plate, filler, the following retaining of 0.22 μ m sieve plate etc. on column piston, transparent polyethylene cylinder, the 0.22 μ m.
Extraction agent is the acid chromatographically pure chemistry reagent with extraction effect.Spreading agent and cleanser are white particle or mixture of powders.The purification filler is housed in the disposable filtering device, purifies filler and can be florisil silica, C18 or Graphon.
The preparation of kit:
The preparation of extraction agent:
Prepare the saturated acetonitrile solution 10mL of 0.5% glacial acetic acid mixing normal hexane, be transferred in the 50mL tool plug screw top polypropylene centrifuge tube.
The preparation of spreading agent
Take by weighing 2g sodium chloride and fully mix, be transferred in the 15mL tool plug screw top polypropylene centrifuge tube with the 5g anhydrous magnesium sulfate.
The preparation of cleanser
Take by weighing the 300mg anhydrous magnesium sulfate and 200mg PSA fully mixes, be transferred in the 15mL tool plug screw top polypropylene centrifuge tube.
Disposable needle tube type filtrator preparation:
In the disposable needle tube type filtrator purification filler is housed, can selects different types of purification filler according to different sample substrates, florisil silica, C18 and Graphon etc. all can be used as the purification filler.Select appropriate filler effectively to purify, can be used as the filler of common fruits and vegetables class sample, and florisil silica and C18 or Graphon make up the filler that can be used as complex samples such as onion, garlic etc. as florisil silica to the fruits and vegetables extract.Disposable needle tube type filtrator is made by oneself by the laboratory, and its cylinder can use repeatedly.
Disposable needle tube type filtrator filling process is: at the sieve plate of syringe bottom pad last layer 0.22 μ m, add filler earlier, cover the sieve plate of one deck 0.22 μ m on filler top again.
Embodiment 2
Application implementation:
1, get dinitroaniline herbicide selective enrichment pretreatment reagent kit in the fruits and vegetables class sample, the inside is furnished with extraction agent, spreading agent, cleanser and disposable needle tube type filtrator.
2, extraction agent, the fruits and vegetables class that contains dinitroaniline herbicide are pulverized sample and spreading agent mixes, shake well obtains mixed solution; The centrifugal 5min of 5000r/min, supernatant is transferred in the cleanser, leave standstill 10min behind the shake well, the dinitroaniline material deposits sample plasma bottle air feed phase chromatogram tandem mass spectrum (GC-MS/MS) in and measures in the described mixed solution after 0.22 μ m one-shot injector formula filtration unit filters, extraction recovery reaches 78.5~109.3% as a result, meets the agricultural residual mensuration requirement of country.
3, test with the sample of matrix more complicated such as onion, with 2 operations down, sample solution injects GC-MS/MS to be measured, and extraction recovery reaches 68.8~102.3% as a result, meets the agricultural residual mensuration requirement of country.
Claims (6)
1. the residual pretreatment reagent kit of dinitroaniline herbicide in the fruits and vegetables, it is characterized in that: kit comprises extraction agent, spreading agent, cleanser centrifuge tube and needle tube type filtrator, extraction agent, spreading agent, cleanser centrifuge tube are tool plug screw top polypropylene centrifuge tube, the needle tube type filtrator is made of column piston, tygon cylinder, retaining sieve plate, filler is housed down in the tygon cylinder from the bottom to top and goes up the retaining sieve plate.
2. according to the residual pretreatment reagent kit of dinitroaniline herbicide in the described fruits and vegetables of claim 1, it is characterized in that: it is 40-60mL that extraction agent centrifuge tube capacity is housed; Spreading agent is housed and cleanser centrifuge tube capacity is 15-20mL.
3. according to the residual pretreatment reagent kit of dinitroaniline herbicide in the described fruits and vegetables of claim 1, it is characterized in that: on keep off sieve plate and down the screen size of retaining sieve plate be 0.15-0.3 μ m.
4. according to the residual pretreatment reagent kit of dinitroaniline herbicide in the described fruits and vegetables of claim 1, it is characterized in that: filler is that florisil silica, C18 or Graphon purify filler.
5. according to the residual pretreatment reagent kit of dinitroaniline herbicide in the described fruits and vegetables of claim 1, it is characterized in that: extraction agent is acid chromatographically pure chemistry reagent.
6. according to the residual pretreatment reagent kit of dinitroaniline herbicide in the described fruits and vegetables of claim 1, it is characterized in that: spreading agent and cleanser are white particle or mixture of powders.
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CN2010206387689U CN201903472U (en) | 2010-12-02 | 2010-12-02 | Pretreatment reagent kit for dinitroaniline herbicide residues in fruit and vegetables |
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CN2010206387689U CN201903472U (en) | 2010-12-02 | 2010-12-02 | Pretreatment reagent kit for dinitroaniline herbicide residues in fruit and vegetables |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102692468A (en) * | 2012-05-22 | 2012-09-26 | 天津出入境检验检疫局动植物与食品检测中心 | Reagent kit for detecting pretreatment of common bactericide in perilla leaf, and method thereof |
CN103091150A (en) * | 2012-11-13 | 2013-05-08 | 中国农业科学院农业质量标准与检测技术研究所 | Multifunctional needle type filter |
CN104181257A (en) * | 2014-08-29 | 2014-12-03 | 福建中烟工业有限责任公司 | Method and composition for extracting and purifying hymexazol pesticide residues in tobacco |
CN109932461A (en) * | 2019-01-31 | 2019-06-25 | 刘军虎 | A kind of pesticide residue method in QuEChERS pretreatment technology combination gas Chromatographic Determination tealeaves |
CN110470808A (en) * | 2018-05-11 | 2019-11-19 | 中国石油化工股份有限公司 | Water quality many reference amounts detection device and detection method based on manual injector |
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2010
- 2010-12-02 CN CN2010206387689U patent/CN201903472U/en not_active Expired - Fee Related
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102692468A (en) * | 2012-05-22 | 2012-09-26 | 天津出入境检验检疫局动植物与食品检测中心 | Reagent kit for detecting pretreatment of common bactericide in perilla leaf, and method thereof |
CN103091150A (en) * | 2012-11-13 | 2013-05-08 | 中国农业科学院农业质量标准与检测技术研究所 | Multifunctional needle type filter |
CN104181257A (en) * | 2014-08-29 | 2014-12-03 | 福建中烟工业有限责任公司 | Method and composition for extracting and purifying hymexazol pesticide residues in tobacco |
CN104181257B (en) * | 2014-08-29 | 2016-04-13 | 福建中烟工业有限责任公司 | Extraction and purification methods and the composition therefor of mould clever residues of pesticides is disliked in tobacco |
CN110470808A (en) * | 2018-05-11 | 2019-11-19 | 中国石油化工股份有限公司 | Water quality many reference amounts detection device and detection method based on manual injector |
CN109932461A (en) * | 2019-01-31 | 2019-06-25 | 刘军虎 | A kind of pesticide residue method in QuEChERS pretreatment technology combination gas Chromatographic Determination tealeaves |
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Granted publication date: 20110720 Termination date: 20111202 |