CN108051511A - The detection method of phenols pesticide in a kind of tealeaves - Google Patents
The detection method of phenols pesticide in a kind of tealeaves Download PDFInfo
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- CN108051511A CN108051511A CN201711197126.2A CN201711197126A CN108051511A CN 108051511 A CN108051511 A CN 108051511A CN 201711197126 A CN201711197126 A CN 201711197126A CN 108051511 A CN108051511 A CN 108051511A
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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
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The present invention relates to a kind of detection methods of phenols pesticide in tealeaves, belong to technical field of food detection.By the use of magnetic ionic liquids as extractant, with reference to Magnetic Isolation, phenols pesticide residue in rapid extraction, analysis tealeaves, establishes tealeaves magnetic ionic liquids dispersive liquid-liquid microextraction analysis method, can expand to the analysis application of other pesticide residues in tealeaves for the first time.
Description
Technical field
The present invention relates to a kind of detection method of phenols pesticide in tealeaves, more particularly to 2,4- dinitro-o-cresols and Te Le
The detection of phenol, belongs to technical field of food detection.
Background technology
Pesticide Residues in Tea brings serious threat to human life's property, and according to statistics, China has 100,000 or so every year
Probably there is 3,000,000 pesticide poisoning event in people's pesticide poisoning, the world every year.Pesticide residue from tea harm to the human body according to
Degree is unusual to be divided into three kinds of acute poisoning, slow poisoning and savings property poisoning.China is tea-drinking big country, due to Pesticides in Tea
Being poisoned caused by medicine residual may all occur at any time.More allow people worried, if pesticide retains too long in human body,
Slow poisoning may be triggered.Improve China's trace standard of pesticide, produce green tea beverage be following tealeaves development it is necessary it
Road.
2,4- dinitro-o-cresols（CA registration numbers：534-52-1）And dinoterb（CA registration numbers：1420-07-1）All it is to use
In pesticide herbicide, sucking is taken in or can be poisoned after skin absorbs, by thermal decomposition liberating nitrogen oxidant smog.It there is no at present
The method being preferably detected to the phenol-derivative herbicide in tealeaves.
The content of the invention
The present invention is using magnetic particle liquid, dispersive liquid-liquid microextraction, High Performance Liquid Chromatography/Mass Spectrometry/mass spectrum (HPLC-MS/
MS) technology establishes the analysis method of 2, the 4- dinitro-o-cresols and dinoterb in tealeaves, and to the commercially available tealeaves in part
It is analyzed.This method can be operated at room temperature, easy, quick.
The detection method of phenols pesticide, includes the following steps in a kind of tealeaves：
1st step after tealeaves sample is ground to powder, adds in n-hexane, is uniformly mixed and then adds in magnetic ionic liquids, into
Row vortex extraction；
2nd step, the mixture that the 1st step obtains carry out centrifugal treating, remove n-hexane layer, add strippant and Fe3O4It receives
Rice corpuscles is stripped by being vortexed extraction；
3rd step, the mixture that the 2nd step obtains carry out centrifugal treating, and the magnetic ionic liquids of centrifuge container bottom are held with magnet,
Take supernatant；
Solvent in supernatant is evaporated and then is dissolved with methanol by the 4th step, is sent into Liquid Chromatography-Tandem Mass Spectrometry instrument to 2,
4- dinitro-o-cresols and dinoterb are analyzed.
The magnetic ionic liquids are selected from [C4MIM][ FeCl4], [C6MIM][ FeCl4] or [C8MIM][
FeCl4] in one or several kinds of mixing.
In 1st step, the volume ratio range of tealeaves and n-hexane is 1：10~30, the addition body of magnetic ionic liquids
Product is the 0.1~1% of n-hexane volume, and the time for being vortexed extraction is 0.5~5min.
In in 2nd step, one or several kinds of mixing of the strippant in；The time of vortex extraction is 1
~5min；Fe3O4The weight of nano-particle is the 1~10% of Tea Samples weight.
The liquid chromatographic detection parameter of the Liquid Chromatography-Tandem Mass Spectrometry instrument is：Using C18Chromatographic column, mobile phase A are
Water containing 0.01 % ammonium hydroxide, Mobile phase B are methanol；Gradient elution program：First the mobile phase A ratio in mobile phase is existed
By 65 % linear reductions to 10 % in 1min, 2 min are kept, then again increase to mobile phase A proportional linearity in 0.1 min
65 % keep 2 min.
The mass spectrograph detection parameters of the Liquid Chromatography-Tandem Mass Spectrometry instrument are：4500 V of spray voltage, atomization gas pressure
50 Psi, 550 DEG C of ion source temperature, 100 ms of sweep time, collision cell exit potential 3.0V, collision cell entrance potential 10. 0
V。
Advantageous effect
By the use of magnetic ionic liquids as extractant, with reference to Magnetic Isolation, rapid extraction analyzes 2,4- dinitro os in tealeaves
Cresols and dinoterb establish magnetic ionic liquids dispersive liquid-liquid microextraction analysis method, can expand to Pesticides in Tea for the first time
The analysis application of medicine.
Description of the drawings
Fig. 1 is influence figure of the ionic liquid species to testing result；
Fig. 2 is influence figure of the ionic liquid dosage to testing result；
Fig. 3 is influence figure of the extraction time species to testing result；
Fig. 4 is the influence figure for extracting accelerating agent species to testing result；
Fig. 5 is influence figure of the strippant species to testing result.
Specific embodiment
The present invention is described in further detail below by specific embodiment.But those skilled in the art will manage
Solution, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Specific skill is not specified in embodiment
Art or condition person carry out according to the described technology of document in the art or condition or according to product description.Examination used
Production firm person is not specified in agent or instrument, and being can be with conventional products that are commercially available.Approximate language used herein is whole
It can be used for modifying any quantity statement in a specification and claims, its relevant basic function can not caused to occur
Permit being changed under conditions of variation.Therefore, the value modified by term such as " about " is not limited to specified accurate
Value.In at least some cases, approximate language can be corresponding with for measuring the precision of the instrument of the value.Unless context or sentence
In indicate otherwise, otherwise range limit can be combined and/or exchange, and this scope be confirmed as and including herein
Included all subranges.In addition to being indicated in the operation embodiment or elsewhere, specification and claims
Used in the amounts of all expression compositions, the number of reaction condition etc. or expression shall be construed as in all cases by
To the modification of word " about ".Word " comprising " used herein, "comprising", " having " or its any other variant are intended to cover non-
It is exclusive including.Technique, method, article or the equipment for e.g., including listing element are not necessarily limited by those elements, but can
This technique, method, article or the intrinsic element of equipment are not explicitly listed or belong to include other.It is expressed with range format
Value should be interpreted as not only including the numerical value as range limit that clearly includes in a flexible way, but also including culvert
All single numbers in the range or subinterval are covered, just as each numerical value and subinterval are expressly recited out.It is for example, " big
About 0.1% to about 5% " concentration range should be understood to the concentration for not only including about 0.1% to about 5% clearly included, also wrap
Include the single concentration in the range of alluding to（Such as, 1%, 2%, 3% and 4%）And subinterval（For example, 0.1% to 0.5%, 1% to 2.2%,
3.3% to 4.4%）.
Instrument and reagent employed in following embodiment：
Instrument
UPLC-3200QTRAP Liquid Chromatography-Tandem Mass Spectrometry instrument（Waters, US's Ultra Performance Liquid Chromatography instrument, American AB I are public
Take charge of triple level Four bar tandem ion-trap mass spectrographs）；Avanti J-26XP refrigerated centrifuges (Beckman companies of the U.S.)；
3 vortex instruments of Genius（German IKA companies）；P120H ultrasonic cleaning machines（German Elma companies）.
Reagent
2,4- dinitro-o-cresol (purity>99.8%), nonyl phenol (dinoterb, purity>98.0%) standard items (Germany
Dr. Ehrenstorfer companies), magnetic ionic liquids [C4MIM][ FeCl4], [C6MIM][ FeCl4] and [C8MIM][
FeCl4]（Upper marine origin victory Chemical Co., Ltd., purity> 98.0%）, Fe3O4Nano-particle（Aladdin company, purity>99.5%,
Specification：20 nm）Methanol, acetonitrile, n-hexane, dichloromethane, petroleum ether, ether, paraxylene are the chromatographically pure (U.S.
Fisher companies), other reagents are pure to analyze.Deionized water is by GenPure UV-TOC/UF × CAD plus（The U.S.
Thermo companies）It is prepared by Superpure water machine.
Detection method is as follows with parameter：
Standard solution is prepared
10 mg2,4- dinitro-o-cresols and dinoterb standard items are weighed respectively, with ethyl alcohol dissolving and 100 mL browns of constant volume
As storing solution in volumetric flask, saved backup in 4 DEG C of refrigerators.Before use, diluting above-mentioned standard stock solution with ethyl alcohol, match somebody with somebody
The standard working solution of various concentration is made, is preserved under the conditions of 4 DEG C.The mixed standard solution of various concentration is now with the current.
Chromatographic condition
Chromatographic column：BEH-C18Chromatographic column（50 mm×2.1 mm, 1.7）；Column temperature：35 ℃；Sample size：5 μL；Flowing
Phase：Mobile phase A is water (containing 0.01 % ammonium hydroxide), and Mobile phase B is methanol, and flow velocity is 0.3 mL/ min；Gradient elution journey
Sequence：10 % A are linearly reduced in 65 % A, 1 min, 2 min is kept, 65 % is then increased linearly in 0.1 min
A keeps 2 min.
Mass Spectrometry Conditions
Ion source：Electric spray ion source（ESI）；Scan mode：Anion scans；Quantitative detection mode:MRM patterns；EFI
Mist voltage（IS）: 4500 V；Atomization gas pressure（GS1）: 50 Psi；Assist gas pressure power（GS2）: 55 Psi；Gas curtain atmospheric pressure
（CUR）：25 Psi；Collision gas（CAD）: Medium；Ion source temperature (TEM): 550 ℃；Sweep time: 100 ms；
Collision cell exit potential（CXP）: 3. 0 V；Collision cell entrance potential（EP）: 10. 0 V；Qualitative ion pair, quota ion
To, collision gas energy（CE）And cluster voltage (DP) is gone to be shown in Table 1.
1 2,4- dinitro-o-cresols of table and dinoterb mass spectrum acquisition parameter
* quota ion
The screening of 1 magnetic particle class of liquids of embodiment
0.5 g of Tea Samples accurately is weighed in 10 mL taper ground glass centrifuge tubes, adds in 10 mL n-hexanes, is vortexed mixed
Even 1. 0 min adds in 50 μ L magnetic particle liquid（[C is respectively adopted6MIM][ FeCl4]、[C4MIM][ FeCl4] and
[C8MIM][ FeCl4]）, 3. 0 min of extraction of ocean eddies centrifuges 5. 0 min with 2000 r/min, removes n-hexane layer, then add
Enter 1 mL paraxylene and 20 mg Fe3O4Nano-particle vortex 2 min back extraction, with 2000 r/min after the completion of back extraction
5. 0 min are centrifuged, magnetic ion liquid is adsorbed in centrifugation bottom of the tube with strong magnet, supernatant is transferred to another glass centrifuge tube
In, repeat above-mentioned paraxylene back extraction process（It is not added with Fe3O4Nano-particle）, merge and be stripped paraxylene supernatant twice,
The dissolving of 0.5 mL methanol is added in after 45 DEG C of nitrogen protection dryings, with sample introduction is analyzed after 0.22 μm of membrane filtration.Magnetic particle liquid
Influence of the body species to extraction efficiency is as shown in Figure 1：Magnetic particle liquid [C6MIM][ FeCl4] to two kinds of environmental estrogens
Extraction efficiency is higher than [C4MIM][ FeCl4] and [C8MIM][ FeCl4]。
The screening of 2 ionic liquid dosage of embodiment
0.5 g of Tea Samples accurately is weighed in 10 mL taper ground glass centrifuge tubes, adds in 10 mL n-hexanes, is vortexed mixed
Even 1. 0 min is separately added into 30,50,80,100,120 μ L magnetic particle liquid [C6MIM][ FeCl4], extraction of ocean eddies 3.
0 min centrifuges 5. 0 min with 2000 r/min, removes n-hexane layer, add 1 mL paraxylene and 20 mg Fe3O4
Nano-particle vortex 2 min back extraction, centrifuges 5. 0 min with 2000 r/min after the completion of back extraction, is being centrifuged with strong magnet
Bottom of the tube adsorbs magnetic ion liquid, and supernatant is transferred in another glass centrifuge tube, repeats above-mentioned paraxylene and was stripped
Journey（It is not added with Fe3O4Nano-particle）, merge and be stripped paraxylene supernatant twice, 0.5 is added in after 45 DEG C of nitrogen protection dryings
ML methanol dissolves, with sample introduction is analyzed after 0. 22 μm of membrane filtrations.
The results are shown in Figure 2：With the increase of magnetic particle liquid volume, extraction efficiency in the range of 30~100 μ L
It is corresponding to improve；Extraction efficiency is declined instead when the volume of magnetic ionic liquids reaches 120 μ L.
The screening of 2 extraction time of embodiment
0.5 g of Tea Samples accurately is weighed in 10 mL taper ground glass centrifuge tubes, adds in 10 mL n-hexanes, is vortexed mixed
Even 1. 0 min adds in 100 μ L magnetic particle liquid [C6MIM][ FeCl4], difference 1~5 min of extraction of ocean eddies, with 2000
R/min centrifuges 5. 0 min, removes n-hexane layer, adds 1 mL paraxylene and 20 mg Fe3O4Nano-particle vortex 2
Min is stripped, and 5. 0 min are centrifuged with 2000 r/min after the completion of back extraction, magnetic in centrifugation bottom of the tube absorption with strong magnet
Supernatant is transferred in another glass centrifuge tube by ionic liquid, repeats above-mentioned paraxylene back extraction process（It is not added with Fe3O4Nanometer
Particle）, merge and be stripped paraxylene supernatant twice, add in the dissolving of 0.5 mL methanol after 45 DEG C of nitrogen protection dryings, use
Sample introduction is analyzed after 0. 22 μm of membrane filtrations.
The results are shown in Figure 3.In 1 to 3min, also gradually increased with the growth extraction efficiency of extraction time, work as the time
To reach maximum during 3 min, during 5min, that is, instead the longer time decreases.
The addition that embodiment 3 extracts accelerating agent improves
Extractant is water-soluble magnetic particle liquid selected in this experiment, and individually extraction efficiency is unsatisfactory in tealeaves,
In order to improve extraction efficiency, acetone and ethyl alcohol is selected to be investigated as extraction accelerating agent respectively.
0.5 g of Tea Samples accurately is weighed in 10 mL taper ground glass centrifuge tubes, adds in 10 mL n-hexanes, whirlpool
1. 0 min of mixing is revolved, adds in 100 μ L magnetic particle liquid [C6MIM][ FeCl4], while also add in 300~700 μ L's
Accelerating agent ethyl alcohol is extracted, respectively 3 min of extraction of ocean eddies, 5. 0 min are centrifuged with 2000 r/min, removed n-hexane layer, then add
Enter 1 mL paraxylene and 20 mg Fe3O4Nano-particle vortex 2 min back extraction, with 2000 r/min after the completion of back extraction
5. 0 min are centrifuged, magnetic ion liquid is adsorbed in centrifugation bottom of the tube with strong magnet, supernatant is transferred to another glass centrifuge tube
In, repeat above-mentioned paraxylene back extraction process（It is not added with Fe3O4Nano-particle）, merge and be stripped paraxylene supernatant twice,
The dissolving of 0.5 mL methanol is added in after 45 DEG C of nitrogen protection dryings, with sample introduction is analyzed after 0. 22 μm of membrane filtrations.
As control, parallel test is carried out as extraction accelerating agent using 400 μ L acetone, compared with the second using 400 μ L
During alcohol, peak area improves 33.2%, illustrates to be better than ethyl alcohol using extraction efficiency during acetone.For this purpose, acetone is selected to promote as extraction
It is investigated into agent, and to different extraction accelerator dosages.Extract influence result of the accelerator dosage to extraction efficiency such as
Shown in Fig. 4.
Embodiment 4 is stripped the screening of species
The amount of migration of 2,4- dinitro-o-cresols and dinoterb in tealeaves is relatively low, in order to meet raising sensitivity for analysis, selection
LC-MS is measured analysis.Magnetic particle liquid is because viscosity and larger, unsuitable direct injection analysis.Therefore, select
Ether, paraxylene, dichloromethane, petroleum ether four kinds of different back washing agents are to two kinds of phenols rings of magnetic particle liquid adsorption
Border estrogen is stripped.
0.5 g of Tea Samples accurately is weighed in 10 mL taper ground glass centrifuge tubes, adds in 10 mL n-hexanes, whirlpool
1. 0 min of mixing is revolved, adds in 100 μ L magnetic particle liquid [C6MIM][ FeCl4], while the extraction for also adding in 500 μ L promotees
Into agent ethyl alcohol and propyl alcohol, 3 min of extraction of ocean eddies, 5. 0 min are centrifuged with 2000 r/min respectively, are removed n-hexane layer, then are added
Enter 1 mL difference strippants（Ether, paraxylene, dichloromethane, petroleum ether）With 20 mg Fe3O4Nano-particle vortex 2
Min is stripped, and 5. 0 min are centrifuged with 2000 r/min after the completion of back extraction, magnetic in centrifugation bottom of the tube absorption with strong magnet
Supernatant is transferred in another glass centrifuge tube by ionic liquid, repeats above-mentioned paraxylene back extraction process（It is not added with Fe3O4Nanometer
Particle）, merge and be stripped paraxylene supernatant twice, add in the dissolving of 0.5 mL methanol after 45 DEG C of nitrogen protection dryings, use
Sample introduction is analyzed after 0. 22 μm of membrane filtrations.
The results are shown in Figure 5 for influence of the strippant species to extraction efficiency.Paraxylene is to 2,4- dinitro-o-cresols
It is better than other three kinds of back washing agents with the effect of extracting of dinoterb.
Methodological study
Under optimal experiment condition, 2,4- dinitro-o-cresols and dinoterb in a kind of new quantitative analysis tealeaves are established
Analysis method.The performance of method for building up in order to evaluate, respectively to working curve, the range of linearity, related coefficient, detection limit and fixed
Amount limit and repeatability are investigated.Selection mark-on sample carries out analysis measure.The reappearance use of this extracting process is smart in the daytime
Density and withinday precision data are assessed.
The range of linearity and quantitative limit
The serial hybrid standard working solution of 2 kinds of object various concentrations is prepared respectively, with target components peak area to respective concentration
Carry out linear regression, using the signal-to-noise ratio of testing compound chromatographic peak in mark-on sample as 3 times of noise signal when corresponding quilt
The concentration value for surveying object calculates detection limit (LODs), the results are shown in Table 2.
2 2,4- dinitro-o-cresols of table and the linear of dinoterb method, precision, detection limit
The rate of recovery and precision of method
In 3 kinds of different tealeaves（Dragon Well tea, Iron Guanyin, Mao Feng）Different amounts of mixed standard solution, 2,4- dinitros are added in matrix
The horizontal mark-on of o-cresol and dinoterb is respectively 0.2,1.0 and 10 μ g/ kg, and each level is repeated 6 times.
0.5 g of Tea Samples accurately is weighed in 10 mL taper ground glass centrifuge tubes, adds in 10 mL n-hexanes, whirlpool
1. 0 min of mixing is revolved, adds in 100 μ L magnetic particle liquid [C6MIM][ FeCl4], while the extraction for also adding in 500 μ L promotees
Into agent ethyl alcohol and propyl alcohol, 3 min of extraction of ocean eddies, 5. 0 min are centrifuged with 2000 r/min respectively, are removed n-hexane layer, then are added
Enter 1 mL strippants paraxylene and 20 mg Fe3O4Nano-particle vortex 2 min back extraction, with 2000 after the completion of back extraction
R/min centrifuges 5. 0 min, adsorbs magnetic ion liquid in centrifugation bottom of the tube with strong magnet, supernatant is transferred to another glass
In centrifuge tube, above-mentioned paraxylene back extraction process is repeated（It is not added with Fe3O4Nano-particle）, merge and be stripped paraxylene twice
Supernatant adds in the dissolving of 0.5 mL methanol, with sample introduction is analyzed after 0. 22 μm of membrane filtrations after 45 DEG C of nitrogen protection dryings.
The rate of recovery and relative standard deviation of relative target object are calculated, the results are shown in Table 3.
The rate of recovery and relative standard deviation of 2 kinds of target compounds in 3 tealeaves of table（n=6）
Claims (6)
1. the detection method of phenols pesticide in a kind of tealeaves, which is characterized in that include the following steps：
1st step after tealeaves sample is ground to powder, is uniformly mixed and then adds in magnetic ionic liquids, carry out vortex extraction；
2nd step, the mixture that the 1st step obtains carry out centrifugal treating, remove n-hexane layer, add strippant and Fe3O4Nanometer
Particle is stripped by being vortexed extraction；
3rd step, the mixture that the 2nd step obtains carry out centrifugal treating, and the magnetic ionic liquids of centrifuge container bottom are held with magnet,
Take supernatant；
Solvent in supernatant is evaporated and then is dissolved with methanol by the 4th step, is sent into Liquid Chromatography-Tandem Mass Spectrometry instrument to 2,
4- dinitro-o-cresols and dinoterb are analyzed.
2. the detection method of phenols pesticide in tealeaves according to claim 1, which is characterized in that the magnetic ion liquid
Body is selected from [C4MIM][ FeCl4], [C6MIM][ FeCl4] or [C8MIM][ FeCl4] in one or several kinds of mixing.
3. the detection method of phenols pesticide in tealeaves according to claim 1, which is characterized in that in the 1st step, tea
The volume ratio range of leaf and n-hexane is 1：10~30, the addition volume of magnetic ionic liquids is the 0.1~1% of n-hexane volume,
The time of vortex extraction is 0.5~5min.
4. the detection method of phenols pesticide in tealeaves according to claim 1, which is characterized in that in the 2nd step,
One or several kinds of mixing of the strippant in；The time of vortex extraction is 1~5min；Fe3O4The weight of nano-particle
It is the 1~10% of Tea Samples weight.
5. the detection method of phenols pesticide in tealeaves according to claim 1, which is characterized in that the liquid chromatogram string
Joining mass spectrometric liquid chromatographic detection parameter is：Using C18Chromatographic column, mobile phase A are the water containing 0.01 % ammonium hydroxide, are flowed
Phase B is methanol；Gradient elution program：First by the mobile phase A ratio in mobile phase in 1min by 65 % linear reductions to 10 %,
2 min are kept, mobile phase A proportional linearity is then increased into 65 % in 0.1 min again, keep 2 min.
6. the detection method of phenols pesticide in tealeaves according to claim 1, which is characterized in that the liquid chromatogram string
Joining mass spectrometric mass spectrograph detection parameters is：4500 V of spray voltage, 50 Psi of atomization gas pressure, 550 DEG C of ion source temperature,
100 ms of sweep time, collision cell exit potential 3.0V, 10. 0 V of collision cell entrance potential.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108586458A (en) * | 2018-05-22 | 2018-09-28 | 四川大学 | A method of tealeaves tea polyphenols and caffeine are detached using ionic liquid extract |
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