CN108645926A - The remaining detection method of pesticide in a kind of Bee Pollen - Google Patents
The remaining detection method of pesticide in a kind of Bee Pollen Download PDFInfo
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- CN108645926A CN108645926A CN201810373005.7A CN201810373005A CN108645926A CN 108645926 A CN108645926 A CN 108645926A CN 201810373005 A CN201810373005 A CN 201810373005A CN 108645926 A CN108645926 A CN 108645926A
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- G—PHYSICS
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- 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
- G01N30/14—Preparation by elimination of some components
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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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
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Abstract
It is to be pre-processed with the following method to Bee Pollen to be measured the present invention relates to the remaining detection method of pesticide, main improvements in a kind of Bee Pollen：1) pesticide residue in Bee Pollen to be measured is fully extracted with acetonitrile, obtains the acetonitrile solution dissolved with pesticide residue；2) acetonitrile solution dissolved with pesticide residue is placed to 3~8min under the conditions of 75~80 DEG C, removes lipid material therein；3) acetonitrile solution for removing lipid material is purified by decontaminating column, must waits for test sample.By the optimization to pesticide Residue analysis method in Bee Pollen, the pesticide residue that can fully extract in Bee Pollen extracts the present invention, lays the foundation for subsequent accurate detection, the present invention has advanced optimized detection method, it can be achieved that accurate must detect.
Description
Technical field
The present invention relates to liquid chromatographic detection technical fields, and in particular to the detection of common pesticide residue in Bee Pollen.
Background technology
Currently, less about the remaining analysis method of Multiple Pesticides in Bee Pollen, the method for report is that major part is used for examining
Survey anabasine pesticide residue.But since honeybee beehive is exposed to around how remaining crop, and it can be also used in honeycomb
His pesticide such as acaricide and fungicide is to reduce the harm of mite class and microsporidian.Statistics indicate that there are various concentration water in honeycomb
Flat insecticide, fungicide and herbicide residue.Therefore, it is necessary to develop a kind of simple, sensitive common pesticides retention analysis
Method.
Since lipid (10-20%) and protein (30-40%) abundant in Bee Pollen can interfere the measurement of retention analysis,
Therefore, if thinking accurately to measure the pesticide residue in Bee Pollen, inherent chaff interferent in Bee Pollen can efficiently be removed by finding one kind
The pre-treating method of (lipid and protein) is premise, determines that appropriate chromatographic test strip part is the key that successfully to detect.
Invention content
The object of the present invention is to provide the remaining detection methods of pesticide in a kind of Bee Pollen, are examined to Bee Pollen to be measured
Before survey, it is pre-processed as follows：
1) pesticide residue in Bee Pollen to be measured is fully extracted with acetonitrile, obtains the acetonitrile solution dissolved with pesticide residue；
2) acetonitrile solution dissolved with pesticide residue is placed to 3~8min under the conditions of -75~-80 DEG C, removes it
In lipid material；
3) acetonitrile solution for removing lipid material is purified by decontaminating column, must waits for test sample.
Also there is the technical solution extracted to the pesticide residue in Bee Pollen using acetonitrile in the prior art, but usually
It is only capable of extracting one or two kinds of pesticide residues, it, can be by 9 kinds of common pesticide residues in Bee Pollen using above-mentioned preprocess method
Carbendazim, Diacloden, clothianidin, imidacloprid, Acetamiprid, Triadimenol, Fluoxastrobin, Resistox and chlopyrifos are carried out at the same time fully
Extraction, the loss of pesticide residue is smaller, and lipid and protein-based interference impurity are few in extracting solution, adequately detect 9
The common pesticide residue of kind lays the foundation.
Preferably, the step 1) is specially：First the Bee Pollen is dissolved in the water, obtains the aqueous solution of Bee Pollen, so
Acetonitrile is added in the aqueous solution of the Bee Pollen afterwards, carries out obtaining the acetonitrile solution dissolved with pesticide residue after fully extracting；
It is further preferred that including the following steps：
A, Bee Pollen to be measured and water are pressed into mass volume ratio 1:It is sufficiently stirred after 2~3 mixing, Bee Pollen is made to be completely dissolved in
In water, the aqueous solution of Bee Pollen is obtained；
B, by the mass volume ratio 1 of Bee Pollen to be measured and acetonitrile:2.5~10, acetonitrile is added to the water of the Bee Pollen
In solution, mixed solution is obtained, the mixed solution is ultrasonically treated, layered shaping is then carried out, takes acetonitrile layer to get molten
Solution has the acetonitrile solution of pesticide residue.
Preferably, the freezing conditions in the step 2) are that 3~5min is freezed under conditions of -80 DEG C.
Preferably, the cleanser is PSA, C18, GCB or Cleanert NANO CARB (m-PFC).
Further preferred Cleanert NANO CARB.It, can be to the impurity in extracting solution by the purified treatment of decontaminating column
It is effectively removed.
Preferably, the mass volume ratio of the Bee Pollen to be measured and acetonitrile is 1:6~8.In the case of above-mentioned amount ratio
Adequately extraction can be achieved and the waste of acetonitrile will not be brought.
Preferably, the condition of the supersound process is that 15~25min is handled under the ultrasound condition that power is 100W.Upper
It is ultrasonically treated under the conditions of stating, the pesticide residue in pollen to be measured can fully be extracted, significantly improve the extraction of solvent
Efficiency.
Preferably, it is ultrasonically treated after completing into the mixed solution plus salt makes its layering.
It is further preferred that the salt is sodium chloride or magnesium sulfate.Prepare liquid can be removed by carrying out layering by addition salt
In moisture or so that water phase and acetonitrile organic phase is kept completely separate, ensure target agricultural chemical compound be leached into acetonitrile organic phase completely
In, then significantly improve the rate of recovery of pesticide.
It is further preferred that during operation, by sample by purifying column purification 2 times.
As a preferred option, the pretreatment of the sample includes the following steps：
1) Bee Pollen to be measured and water are pressed into mass volume ratio 1:Being sufficiently stirred after 2~3 mixing makes Bee Pollen be completely dissolved in
In water, the aqueous solution of Bee Pollen is obtained；By the mass volume ratio 1 of Bee Pollen to be measured and acetonitrile:6~8, acetonitrile is added to the bee
In the aqueous solution of pollen, obtain mixed solution, to the mixed solution power be 100W ultrasound condition under processing 15~
25min adds sodium chloride or magnesium sulfate that mixed liquor is made to be layered, and takes the acetonitrile layer dissolved with pesticide residue；
2) acetonitrile layer dissolved with pesticide residue under the conditions of -80 DEG C is placed into 4min, removes lipid therein
Matter；
3) it uses decontaminating column Cleanert NANO CARB to purify the acetonitrile solution for removing lipid material 2 times, must wait for test sample.
Preferably, the step of being detected to Bee Pollen to be measured by liquid chromatography is as follows：
1) Bee Pollen to be measured is pre-processed, obtains and described waits for test sample；
2) wait for that test sample is detected to described by liquid chromatogram, select volume fraction for 0.1% formic acid aqueous solution
For mobile phase A, the acetonitrile solution for the formic acid that volume fraction is 0.1% is Mobile phase B, and gradient elution is carried out to Bee Pollen to be measured；
During gradient elution, the volume fraction of 0~3min, Mobile phase B increase to 50% by 30%；3-5min, stream
The volume fraction of dynamic phase B increases to 75% by 50%；The volume fraction of 5-6min, Mobile phase B increase to 90% by 75%；6-
The volume fraction of 11min, Mobile phase B maintain 90%.
Under above-mentioned testing conditions, can to the obtained 9 kinds of common pesticides of extraction, carbendazim, Diacloden, clothianidin,
Imidacloprid, Acetamiprid, Triadimenol, Fluoxastrobin, Resistox and chlopyrifos ideal must detach and detect.
Preferably, the flow velocity of mobile phase is 0.3~0.4mL/min；
Preferably, detector is triple level four bars mass detectors.
It is further preferred that the condition of Mass Spectrometer Method is 340 DEG C, gas flow rate 12L/min of gas temperature, sprayer electricity
Pressure:40psi, capillary voltage:4000V, spray chamber's electric current:1.1 μ A, electron multiplier voltage:400, it can by Mass Spectrometer Method
Effectively improve the response of the sensitivity and target monitoring ion of instrument detection.
The method of the present invention has the advantages that：
1) present invention can be extracted fully common in Bee Pollen by the optimization to pesticide Residue analysis method in Bee Pollen
9 kinds of pesticide residues, for it is subsequent it is accurate detection lay the foundation.
2) present invention, can be to common in Bee Pollen by the optimization to liquid chromatographic detection condition and Mass Spectrometer Method condition
Pesticide residue progress is ideal to be detached, and realization accurately detects.
Description of the drawings
The influence of Fig. 1 Extraction solvents 9 kinds of pesticide rate of recovery of volume pair；
The influence of 9 kinds of pesticide rate of recovery of Fig. 2 cooling times pair；
The influence of Fig. 3 cleansers 9 kinds of pesticide rate of recovery of type pair；
The influence of Fig. 4 decontaminating column Cleanert NANO CARB 9 kinds of pesticide rate of recovery of filtering times pair.
Specific implementation mode
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
The present embodiment is related to the remaining detection of pesticide in Bee Pollen, includes the following steps：
A, the pre-treatment of sample
1) it weighs 2g pollen to be measured to be placed in 50mL centrifuge tubes, 5mL pure water is added into centrifuge tube, vortex 1min obtains bee
The aqueous solution of pollen；
2) 15mL acetonitriles are added into the aqueous solution of the Bee Pollen, 20min is extracted under the ultrasound of power 100W, to
Salt packet (sodium chloride or magnesium sulfate) is added in 50mL centrifuge tubes, be vortexed concussion 1min, takes acetonitrile layer；
3) acetonitrile layer is placed into 4min under the conditions of -80 DEG C, 3800rpm, 4 DEG C of centrifugation 5min take supernatant.
4) supernatant is crossed into Cleanert NANO CARB pillars, pushes away altogether 2 times, completes the pre-treatment of sample.
B, chromatography
LC-QQQ-MS/MS analyses are carried out to the sample that pre-treatment is completed.
The condition of liquid-phase chromatographic analysis is：0.5 μ L of sample size；
Flow rate of mobile phase：0.350mL/min；
Mobile phase：A, the acetonitrile of 0.1% formic acid water B of volume fraction, 0.1% formic acid of volume fraction；
The program of gradient elution is：The volume fraction of 0~3min, Mobile phase B increase to 50% by 30%；3-5min, stream
The volume fraction of dynamic phase B increases to 75% by 50%；The volume fraction of 5-6min, Mobile phase B increase to 90% by 75%；6-
The volume fraction of 11min, Mobile phase B maintain 90%.
Mass Spectrometry Conditions are：Gas temperature:340 DEG C, gas flow rate:12L/min, nebulizer pressure:40psi, capillary electricity
Pressure:4000V, 1.1 μ A of spray chamber's electric current, electron multiplier voltage:400.The mass spectrum acquisition parameter of each compound is shown in Table 1.
C, linear equation, detection limit and quantitative limit
The standard items for taking various farm chemical ingredients are configured to a concentration of 100mg L-1Storing solution.Acetonitrile/matrix solution is dilute
Release, it is configured to a concentration of 0.01 respectively, 0.05,0.1,0.5,1,2.5,5mg L-1The hybrid standard of 7 different levels is molten
Liquid, after HPLC-QQQ is measured, using mass concentration as abscissa, peak area is that ordinate establishes standard curve.To add recycling
Sample peak response is the addition density calculating method detection limit (LOD) of 3 times of noises, with the addition concentration calculating side of 10 times of noises
Standard measure limits (LOQ).
The results are shown in Table 2, in 0.01-5mg L-1It is linear good in concentration range, related coefficient ranging from 0.9922-
0.9996, Mechanism and effect ranging from 0-29.29%.The detection limit and quantitative limit of carbendazim are respectively 0.60 and 2.03 μ g/kg, thiophene
Worm piperazine, clothianidin, imidacloprid, Acetamiprid, Triadimenol and Fluoxastrobin detection limit and quantitative limit be respectively 0.75 and 2.63 μ g/
The detection limit and quantitative limit of kg, Resistox and chlopyrifos are respectively 45 and 150 μ g/kg.
19 kinds of the retention time of the compound of table, monitoring ion and collision voltage
Detection line (LOD), quantitative limit (LOQ), linear equation, related coefficient (R2) and the matrix effect of 29 kinds of pesticides of table
It answers (ME)
Note：Matrix effect (%)=(the same amount pesticide response added in sample substrate)/(in pure solvent pesticide
Response) × 100
Experimental example
This experimental example verifies the accuracy of the present processes, in blank rape pollen sample add 150,
The mixed standard solutions of 375 and 750 different levels of μ g/kg 3 carries out rate of recovery experiment, each to add the parallel repetition of concentration 5
It is secondary, calculate the rate of recovery and relative standard deviation (RSD).The results are shown in Table 3, the average mark-on of 9 kinds of pesticides in rape pollen
The rate of recovery is between 82.5%-112.9%, and for relative standard deviation (RSD) between 1.6-10.8%, method has preferable return
Yield and reproducibility.
The sample recovery rate (n=5) and relative deviation (RSD) of 39 kinds of pesticides of table
Comparative example 1
This comparative example is related to the adjustment of extractant volume, compared with Example 1, differs only in, sample pre-treatments
In step 1), the optimization of Extraction solvent acetonitrile volume：5mL, 10mL and 20mL, and compared with the 15mL in embodiment 1,
The result is shown in Figure 1.As shown in Figure 1, when the volume of extractant is 15mL, the determinand content highest extracted.
Comparative example 2
This comparative example is related to the adjustment of cooling time in extraction process, and compared with Example 1, difference lies in before sample
In the step 3) of processing, cooling time is adjusted separately as 0min and 8min, is compared with 4min is freezed in 1 phase of embodiment,
The result is shown in Fig. 2, as shown in Figure 2, when cooling time is 4min, the determinand content highest extracted.
Comparative example 3
This comparative example is related to the adjustment of multi-walled carbon nanotube filterable form decontaminating column in extraction process, compared with Example 1,
Difference lies in the step 4) of pre-treatment, cleanser type is selected respectively：Decontaminating column in PSA, C18, GCB and embodiment 1
Cleanert NANO CARB (m-PFC) are compared, and the result is shown in Fig. 3, from the figure 3, it may be seen that Cleanert NANO CARB (m-
PFC) extraction effect of decontaminating column is best.
Comparative example 4
This comparative example is related to the adjustment of Cleanert NANO CARB solid-phase extraction column numbers, compared with Example 1, area
Be not only that, the number that supernatant crosses Cleanert NANO CARB solid-phase extraction columns is respectively 1 time and 3 times, and with embodiment 1
The operation that middle mistake is 2 times is compared, and the result is shown in Fig. 4.Fig. 4 is it is found that when crossing column 2 times, the determinand content highest extracted.
Although above having used general explanation, specific implementation mode and experiment, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (10)
1. the remaining detection method of pesticide in a kind of Bee Pollen, which is characterized in that before being detected to Bee Pollen to be measured, to it
It is pre-processed as follows：
1) pesticide residue in Bee Pollen to be measured is fully extracted with acetonitrile, obtains the acetonitrile solution dissolved with pesticide residue；
2) acetonitrile solution dissolved with pesticide residue is placed to 3~8min under the conditions of -75~-80 DEG C, removal is therein
Lipid material；
3) acetonitrile solution for removing lipid material is purified by decontaminating column, must waits for test sample.
2. detection method according to claim 1, which is characterized in that the step 1) is specially：
First the Bee Pollen is dissolved in the water, obtains the aqueous solution of Bee Pollen, is then added in the aqueous solution of the Bee Pollen
Acetonitrile carries out obtaining the acetonitrile solution dissolved with pesticide residue after fully extracting；
Preferably, include the following steps：
A, Bee Pollen to be measured and water are pressed into mass volume ratio 1:It is sufficiently stirred after 2~3 mixing, Bee Pollen is made to be completely dissolved in water
In, obtain the aqueous solution of Bee Pollen；
B, by the mass volume ratio 1 of Bee Pollen to be measured and acetonitrile:2.5~10, acetonitrile is added to the aqueous solution of the Bee Pollen
In, obtain mixed solution, the mixed solution be ultrasonically treated, then carry out layered shaping, take acetonitrile layer to get dissolved with
The acetonitrile solution of pesticide residue.
3. detection method according to claim 1 or 2, which is characterized in that the acetonitrile solution dissolved with pesticide residue
3~5min is placed under the conditions of -80 DEG C.
4. according to claims 1 to 3 any one of them detection method, which is characterized in that the cleanser is PSA, C18, GCB
Or Cleanert NANO CARB, preferably Cleanert NANO CARB.
5. according to Claims 1 to 4 any one of them detection method, which is characterized in that the Bee Pollen to be measured and acetonitrile
Mass volume ratio is 1:6~8.
6. according to claim 2~5 any one of them detection method, which is characterized in that the condition of the supersound process be
15~25min is handled under the ultrasound condition that power is 100W；
And/or it is ultrasonically treated after completion and adds salt to make its layering into the mixed solution；Preferably, the salt be sodium chloride or
Magnesium sulfate.
7. detection method according to claim 1, which is characterized in that before being detected to Bee Pollen to be measured, to its into
The following pretreatment of row：
1) Bee Pollen to be measured and water are pressed into mass volume ratio 1:Being sufficiently stirred after 2~3 mixing makes Bee Pollen be completely dissolved in water,
Obtain the aqueous solution of Bee Pollen；By the mass volume ratio 1 of Bee Pollen to be measured and acetonitrile:6~8, acetonitrile is added to the Bee Pollen
Aqueous solution in, obtain mixed solution, to the mixed solution power be 100W ultrasound condition under handle 15~25min, add
Sodium chloride or magnesium sulfate make mixed liquor be layered, and take the acetonitrile layer dissolved with pesticide residue；
2) acetonitrile layer dissolved with pesticide residue under the conditions of -80 DEG C is placed into 4min, removes lipid material therein；
3) it uses decontaminating column Cleanert NANO CARB to purify the acetonitrile solution for removing lipid material 2 times, must wait for test sample.
8. according to claim 1~7 any one of them detection method, which is characterized in that include the following steps：
1) Bee Pollen to be measured is pre-processed, obtains and described waits for test sample；
2) wait for that test sample is detected to described by liquid chromatogram, it for the aqueous solution of 0.1% formic acid is stream to select volume fraction
Dynamic phase A, the acetonitrile solution for the formic acid that volume fraction is 0.1% is Mobile phase B, and gradient elution is carried out to Bee Pollen to be measured；
During gradient elution, the volume fraction of 0~3min, Mobile phase B increase to 50% by 30%；3-5min, Mobile phase B
Volume fraction increase to 75% by 50%；The volume fraction of 5-6min, Mobile phase B increase to 90% by 75%；6-11min,
The volume fraction of Mobile phase B maintains 90%.
9. detection method according to claim 8, which is characterized in that the flow velocity of mobile phase is 0.3~0.4mL/min.
10. detection method according to claim 8 or claim 9, which is characterized in that detector is triple level four bars Mass Spectrometer Methods
Device；Preferably, the condition for Mass Spectrometer Method being carried out using triple level four bars mass detectors is 340 DEG C of gas temperature, gas flow rate
12L/min, spray pressure power:40psi, capillary voltage:4000V, spray chamber's electric current:1.1 μ A, electron multiplier voltage:
400。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113884606A (en) * | 2021-10-22 | 2022-01-04 | 生态环境部南京环境科学研究所 | Method for determining 47 pesticide residues in honey and bee pollen |
| CN113933443A (en) * | 2021-10-27 | 2022-01-14 | 上海市农产品质量安全中心 | In-situ rapid detection method for acetamiprid in vegetables or fruits |
| CN113933446A (en) * | 2021-10-27 | 2022-01-14 | 上海市农产品质量安全中心 | Method for rapidly detecting 10 pyrethroid pesticide residues in situ and kit thereof |
| CN114252311A (en) * | 2021-10-27 | 2022-03-29 | 上海市农产品质量安全中心 | Method for carrying out in-situ rapid detection pretreatment on pesticide residues in vegetables and fruits |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009186435A (en) * | 2008-02-08 | 2009-08-20 | Tsumura & Co | Method of purifying residual agricultural chemicals in herbal medicine sample |
| CN102183611A (en) * | 2011-03-13 | 2011-09-14 | 浙江大学 | Method for detecting pesticide residue in white paeony root crude drug |
| CN103293244A (en) * | 2013-06-06 | 2013-09-11 | 宁波检验检疫科学技术研究院 | Method for measuring residues of seven pesticides in wool fat by liquid chromatography-tandem mass spectrometry |
| CN104931597A (en) * | 2015-01-05 | 2015-09-23 | 深圳出入境检验检疫局食品检验检疫技术中心 | Method capable of simultaneously detecting varieties of pesticide residues in aquatic product |
| CN106324123A (en) * | 2016-08-09 | 2017-01-11 | 国家烟草质量监督检验中心 | Determination method of pesticide residual quantity in tobacco and tobacco products |
| CN106383180A (en) * | 2016-08-19 | 2017-02-08 | 中华人民共和国日照出入境检验检疫局 | A method of detecting a plurality of pesticide residues in silkworm pupae |
| CN107389847A (en) * | 2017-06-05 | 2017-11-24 | 中国农业科学院蜜蜂研究所 | A kind of method of lipid component in quick analysis Bee Pollen |
| CN107478737A (en) * | 2017-07-18 | 2017-12-15 | 贵州茅台酒股份有限公司 | A kind of method of 80 kinds of persticide residues in detection white wine |
-
2018
- 2018-04-24 CN CN201810373005.7A patent/CN108645926B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009186435A (en) * | 2008-02-08 | 2009-08-20 | Tsumura & Co | Method of purifying residual agricultural chemicals in herbal medicine sample |
| CN102183611A (en) * | 2011-03-13 | 2011-09-14 | 浙江大学 | Method for detecting pesticide residue in white paeony root crude drug |
| CN103293244A (en) * | 2013-06-06 | 2013-09-11 | 宁波检验检疫科学技术研究院 | Method for measuring residues of seven pesticides in wool fat by liquid chromatography-tandem mass spectrometry |
| CN104931597A (en) * | 2015-01-05 | 2015-09-23 | 深圳出入境检验检疫局食品检验检疫技术中心 | Method capable of simultaneously detecting varieties of pesticide residues in aquatic product |
| CN106324123A (en) * | 2016-08-09 | 2017-01-11 | 国家烟草质量监督检验中心 | Determination method of pesticide residual quantity in tobacco and tobacco products |
| CN106383180A (en) * | 2016-08-19 | 2017-02-08 | 中华人民共和国日照出入境检验检疫局 | A method of detecting a plurality of pesticide residues in silkworm pupae |
| CN107389847A (en) * | 2017-06-05 | 2017-11-24 | 中国农业科学院蜜蜂研究所 | A kind of method of lipid component in quick analysis Bee Pollen |
| CN107478737A (en) * | 2017-07-18 | 2017-12-15 | 贵州茅台酒股份有限公司 | A kind of method of 80 kinds of persticide residues in detection white wine |
Non-Patent Citations (6)
| Title |
|---|
| KONSTANTINOS M. KASIOTIS 等: "Pesticide residues in honeybees, honey and bee pollen by LC–MS/MS screening: Reported death incidents in honeybees", 《SCIENCE OF THE TOTAL ENVIRONMENT》 * |
| P. PARRILLA VÁZQUEZ 等: "A sensitive and efficient method for routine pesticide multiresidue analysis in bee pollen samples using gas and liquid chromatography coupled to tandem mass spectrometry", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 樊苑牧 等: "快速溶剂萃取-高效液相色谱法测定含脂羊毛中残留的除虫脲和杀铃脲", 《色谱》 * |
| 王多娇 等: "快速SPE-UPLC-MS/MS同时测定茶叶中的5种农药残留", 《江苏农业科学》 * |
| 王思威 等: "高效液相色谱-串联质谱法测定荔枝花粉和花蜜中腈菌唑和苯醚甲环唑残留", 《色谱》 * |
| 许美玲 等: "高效液相色谱-串联质谱法快速测定食品中的抗倒胺残留量", 《色谱》 * |
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| CN113884606A (en) * | 2021-10-22 | 2022-01-04 | 生态环境部南京环境科学研究所 | Method for determining 47 pesticide residues in honey and bee pollen |
| CN113933443A (en) * | 2021-10-27 | 2022-01-14 | 上海市农产品质量安全中心 | In-situ rapid detection method for acetamiprid in vegetables or fruits |
| CN113933446A (en) * | 2021-10-27 | 2022-01-14 | 上海市农产品质量安全中心 | Method for rapidly detecting 10 pyrethroid pesticide residues in situ and kit thereof |
| CN114252311A (en) * | 2021-10-27 | 2022-03-29 | 上海市农产品质量安全中心 | Method for carrying out in-situ rapid detection pretreatment on pesticide residues in vegetables and fruits |
| CN113933446B (en) * | 2021-10-27 | 2024-04-09 | 上海市农产品质量安全中心 | Method for in-situ rapid detection of 10 pyrethroid pesticide residues and kit thereof |
| CN113933443B (en) * | 2021-10-27 | 2024-05-03 | 上海市农产品质量安全中心 | In-situ rapid detection method for acetamiprid in vegetables or fruits |
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