CN109270185A - A kind of the QuChERS method tealeaves pretreatment reagent kit and pre-treating technology of improvement - Google Patents
A kind of the QuChERS method tealeaves pretreatment reagent kit and pre-treating technology of improvement Download PDFInfo
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- CN109270185A CN109270185A CN201811003683.0A CN201811003683A CN109270185A CN 109270185 A CN109270185 A CN 109270185A CN 201811003683 A CN201811003683 A CN 201811003683A CN 109270185 A CN109270185 A CN 109270185A
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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
Abstract
The invention discloses the QuChERS method tealeaves pretreatment reagent kits and pre-treating technology of a kind of improvement, the pretreatment reagent kit includes extracting reagent packet and purification reagent packet, sodium chloride-containing 1g, sodium acetate 1g, anhydrous magnesium sulfate 2g in the extraction reagent packet, containing graphene 0.1g, PSA0.25g, GCB0.1g in the purification reagent packet.The present invention improves detection efficiency, mitigates testing staff's burden, large batch of sample can be made within the unit time；The organic reagents such as acetonitrile, acetone are saved, testing cost is reduced；Reduce contact of the testing staff with organic reagent, protection testing staff's safety.
Description
Technical field
The present invention relates to a set of chemical agent combination, the preceding place of more pesticide residue quantitative detections suitable for Tea Samples
Reason.
Background technique
The Detecting Pesticide of tealeaves is related to the quality safety of tealeaves.Tea Samples matrix is complicated, and interfering substance is more,
Sample pre-treatments are time-consuming longest, workload the best part during Detecting Pesticide, and determine the accurate of analysis method
Degree and precision.QuEChERS (quick, easy, cheap, effective, rugged, safe) method is more as a kind of pesticide
The pre-treating method of retention analysis becomes in recent years due to having the characteristics that quick, simple, cheap, effective, reliable, safe
Research hotspot.For the higher vegetables of water content and fruit when QuEChERS method initial design, and to water content compared with
Limitation is very big for low dry tea product.Huang Cheng etc. (2012) is residual with the pyrethroid pesticide in acetonitrile extraction tealeaves
It stays, chooses N- propyl ethylenediamine (PSA), ODSC18 and Graphon (GCB) and purified, detected using gas-chromatography ECD
Device analysis, it is 78.2-109.0% that gained, which only has 8 kinds of pesticide recovery of standard addition,.Zhang etc. (2014) is using improved
When QuEChERS method analyzes the triazole bactericidal agent residual in tealeaves, using acetonitrile as Extraction solvent, C18, SPA and Fu Luoli silicon
After soil purification, the process of a liquid-liquid micro-extraction is increased, although reducing the interference of matrix, process is relatively cumbersome.Ye Jiang
(2012) team such as thunder (2013) and Lozano extracts to acetonitrile, and PSA and GCB are purified in the technique study combined tealeaves
The residual of Multiple Pesticides, recycled in its entirety rate and matrix interference situation are less desirable, often the high method clean-up effect of the rate of recovery
Bad or good purification the rate of recovery is not high enough.
Summary of the invention
The purpose of the present invention is to provide a kind of QuChERS method tealeaves pretreatment reagent kits of improvement, introduce novel
Nano material graphene is used as cleanser after mixing with PSA, clean-up effect is better than conventional purges such as florisil silica, carbon blacks
Agent, and there is significant advantage in terms of the rate of recovery, more pesticides.
The object of the invention is also to provide a kind of pre-treatment works of the QuChERS method tealeaves pretreatment reagent kit of improvement
Skill improves detection efficiency, mitigates testing staff's burden, large batch of sample can be made within the unit time；Save acetonitrile, acetone
Equal organic reagents, reduce testing cost；Reduce contact of the testing staff with organic reagent, protection testing staff's safety.
The present invention is achieved through the following technical solutions: before the present invention provides a kind of QuChERS method tealeaves of improvement
Kit is managed, including extracts reagent packet and purification reagent packet, it is sodium chloride-containing 1g in the extraction reagent packet, sodium acetate 1g, anhydrous
Magnesium sulfate 2g, containing graphene 0.1g, PSA0.25g, GCB0.1g in the purification reagent packet.
The present invention also provides a kind of pre-treating technologies of the QuChERS method tealeaves pretreatment reagent kit of improvement, including
It extracts and purifies two steps:
It extracts: 10g tealeaves being taken to be placed in the centrifuge tube of 100ml, the acetonitrile that 20ml contains 1% acetic acid is added, seal homogeneous
Centrifuge tube is placed in ice water after 30s, is added and extracts reagent packet, is mixed, ultrasonic extraction 10min, is centrifuged under 5000 turns
10min；
Purification: taking the upper layer 5ml extracting solution to come out, and addition is placed in the 10ml centrifuge tube of ice water, is put into centrifuge tube net
Change reagent packet, homogeneous 1min, 12000 turns/min centrifugation 10min after mixing well takes 3ml supernatant liquid nitrogen to be blown to close dry, uses
1.5ml ethyl acetate dissolved film and carries out gas phase analysis, and remaining scavenging solution crosses film bottling and carries out liquid phase analysis.
Preferably, tealeaves is 100 mesh.
Preferably, supernatant liquid nitrogen is blown to closely dry temperature and is set as 45 DEG C in purifying step.
Compared with prior art, the present invention has the effect that
1. improving detection efficiency, mitigates testing staff's burden, large batch of sample can be made within the unit time；Save second
The organic reagents such as nitrile, acetone reduce testing cost；Reduce contact of the testing staff with organic reagent, protection testing staff's safety.
2. introducing as cleanser after novel nano material graphene is mixed with PSA, clean-up effect is better than Fu Luoli
The conventional purges agent such as tripoli, carbon black, and there is significant advantage in terms of the rate of recovery, more pesticides.
3. detection limit and in terms of be able to satisfy Pesticide Residues in Tea analysis requirement, and cost be lower than quotient
Product matrix scattered adsorption agent.
Detailed description of the invention
It, below will be to required in embodiment or description of the prior art in order to illustrate more clearly of technical solution of the present invention
The attached drawing used is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, right
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings
Its attached drawing.
Fig. 1 be sample addition recycling addition concentration be 0.10mg/kg time gas chromatography mass spectrogram.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art without creative labor it is obtained it is all its
His embodiment, shall fall within the protection scope of the present invention.
One, the QuChERS method tealeaves pretreatment reagent kit improved
Extract reagent packet, the salts substances such as interior sodium chloride-containing 1g, sodium acetate 1g, anhydrous magnesium sulfate 2g, it is ensured that by tea
Pesticide residue inside leaf is by Solid Phase Extraction to liquid phase.
Reagent packet is purified, the adsorbents such as interior containing graphene 0.1g, PSA0.25g, GCB0.1g, combining can be maximum
Degree adsorbs the detection interfering substance in tealeaves.
Wherein, PSA refers to that N- propyl ethylenediamine, GCB refer to Graphon.
Detection interfering substance inside tealeaves is mainly chlorophyll and fatty acid etc., and PSA can effectively remove the rouge of the inside
Fat acid, graphene then have good adsorption effect to chlorophyll.Detection efficiency not only can be improved using graphene and
And testing cost can be substantially reduced.
Two, pre-treating technology, including extract and purify two key steps:
1, it extracts (with reagent packet is extracted): 10g tealeaves (100 mesh) being taken to be placed in the centrifuge tube of 100ml, 20ml is added and contains
Centrifuge tube is placed in ice water by the acetonitrile of 1% acetic acid after sealing homogeneous 30s, is added and is extracted reagent packet, is mixed, ultrasonic extraction
10min is centrifuged 10min under 5000 turns.
Acetic acid-sodium acetate purpose is added and is to maintain extraction solution slant acidity environment, prevents pesticide from decomposing, due to anhydrous sulphur
Sour magnesium meets water heat release, easily leads to pesticide decomposition, therefore is put into ice water.
2, it purification (with reagent packet is purified): takes the upper layer 5ml extracting solution to come out, is added in 10ml centrifuge tube that (centrifuge tube is put
It is placed in ice water), purification reagent packet is put into centrifuge tube, homogeneous 1min, 12000 turns/min centrifugation 10min, takes after mixing well
3ml supernatant liquid nitrogen is blown to closely dry (temperature is set as 45 DEG C), dissolved film with 1.5ml ethyl acetate and carries out gas phase analysis (gas phase
Chromatography, gas chromatography-mass spectrometry), remaining scavenging solution crosses film bottling and carries out liquid phase analysis (liquid chromatogram, liquid chromatogram matter
Compose combined instrument).
Three, result
1, Fig. 1 is sample addition recycling (addition concentration 0.10mg/kg) gaschromatographic mass spectrometry figure (GC-MS-MS), from Fig. 1
In it can be seen that in sample the peak distribution of each parameter it is good, matrix good purification.
2, the various pesticide rate of recovery are shown in Table 1
The various pesticide rate of recovery of table 1
As known from Table 1 by pesticides such as organic phosphorus, organochlorine, pyrethroids respectively with 0.05mg/kg, 0.1mg/kg, 0.5mg/kg
Three concentration add in the sample, obtain the rate of recovery in the 70-130% range of national requirements by machine on pre-treatment extraction and cleaning
Interior, relative standard deviation is respectively less than 20%.
Claims (4)
1. a kind of QuChERS method tealeaves pretreatment reagent kit of improvement, which is characterized in that including extracting reagent packet and purification examination
Agent packet, sodium chloride-containing 1g, sodium acetate 1g, anhydrous magnesium sulfate 2g in the extraction reagent packet, graphitiferous in the purification reagent packet
Alkene 0.1g, PSA0.25g, GCB0.1g.
2. the pre-treating technology for the QuChERS method tealeaves pretreatment reagent kit improved as described in claim 1, feature exist
In, including extract and purify two steps:
It extracts: 10g tealeaves being taken to be placed in the centrifuge tube of 100ml, the acetonitrile that 20ml contains 1% acetic acid is added, after sealing homogeneous 30s
Centrifuge tube is placed in ice water, is added and extracts reagent packet, is mixed, ultrasonic extraction 10min, is centrifuged 10min under 5000 turns；
Purification: taking the upper layer 5ml extracting solution to come out, and addition is placed in the 10ml centrifuge tube of ice water, and purification examination is put into centrifuge tube
Agent packet, homogeneous 1min, 12000 turns/min centrifugation 10min after mixing well take 3ml supernatant liquid nitrogen to be blown to close dry, with 1.5ml second
Acetoacetic ester dissolved film and carries out gas phase analysis, and remaining scavenging solution crosses film bottling and carries out liquid phase analysis.
3. the pre-treating technology for the QuChERS method tealeaves pretreatment reagent kit improved as claimed in claim 2, feature exist
In tealeaves is 100 mesh.
4. the pre-treating technology for the QuChERS method tealeaves pretreatment reagent kit improved as claimed in claim 2, feature exist
In supernatant liquid nitrogen is blown to closely dry temperature and is set as 45 DEG C in purifying step.
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| CN201811003683.0A CN109270185A (en) | 2018-08-30 | 2018-08-30 | A kind of the QuChERS method tealeaves pretreatment reagent kit and pre-treating technology of improvement |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2514828C2 (en) * | 2012-07-11 | 2014-05-10 | Федеральное государственное бюджетное учреждение "Федеральный центр охраны здоровья животных" (ФГБУ "ВНИИЗЖ") | Method of determining mycotoxins in animal and vegetable products |
| CN106324106A (en) * | 2015-06-15 | 2017-01-11 | 财团法人食品工业发展研究所 | Method for distinguishing same tea product from different producing areas |
| CN106770841A (en) * | 2017-03-23 | 2017-05-31 | 西北师范大学 | The method that fruit Pesticides Testing sample is processed using QuEChERS abstraction techniques |
| CN107300598A (en) * | 2017-08-22 | 2017-10-27 | 福建出入境检验检疫局检验检疫技术中心 | It is a kind of to be used for the pre-treating method of Multiple Pesticides residue detection in tealeaves |
-
2018
- 2018-08-30 CN CN201811003683.0A patent/CN109270185A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2514828C2 (en) * | 2012-07-11 | 2014-05-10 | Федеральное государственное бюджетное учреждение "Федеральный центр охраны здоровья животных" (ФГБУ "ВНИИЗЖ") | Method of determining mycotoxins in animal and vegetable products |
| CN106324106A (en) * | 2015-06-15 | 2017-01-11 | 财团法人食品工业发展研究所 | Method for distinguishing same tea product from different producing areas |
| CN106770841A (en) * | 2017-03-23 | 2017-05-31 | 西北师范大学 | The method that fruit Pesticides Testing sample is processed using QuEChERS abstraction techniques |
| CN107300598A (en) * | 2017-08-22 | 2017-10-27 | 福建出入境检验检疫局检验检疫技术中心 | It is a kind of to be used for the pre-treating method of Multiple Pesticides residue detection in tealeaves |
Non-Patent Citations (3)
| Title |
|---|
| WENBI GUAN等: "Graphene as dispersive solidphase extraction materials for pesticides LC-MS/MS multi-residue analysis in leek, onion and garlic", 《FOOD ADDITIVES & CONTAMINANTS: PART A》 * |
| XUE LIU等: "Pesticide Multi-Residue Analysis in Tea Using d-SPE Sample Cleanup with Graphene Mixed with Primary Secondary Amine and Graphitized Carbon Black Prior to LC–MS/MS", 《CHROMATOGRAPHIA》 * |
| 杨永坛等: "气相色谱法快速测定茶叶中有机氯、拟除虫菊酯和有机磷农药残留", 《食品安全质量检测学报》 * |
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