CN106226444A - The high-efficiency liquid chromatography method for detecting of avilamycin content in a kind of edible vegetable oil - Google Patents
The high-efficiency liquid chromatography method for detecting of avilamycin content in a kind of edible vegetable oil Download PDFInfo
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Abstract
The invention discloses the HPLC (high performance liquid chromatography) of avilamycin content in a kind of edible vegetable oil, its by sample through methanol vortex concussion extract after, with ODS C18 Solid-Phase Extraction column purification, with N Methylimidazole. and trifluoroacetic anhydride derivatization, finally it is measured with liquid chromatograph fluorescence method.The reagent that this method uses is less, cost-effective；Sample-pretreating method is simple, and good purification decreases instrument maintenance in use, and when solving use liquid chromatograph UV-detector, sensitivity is the lowest, the technical problem that matrix interference is more serious；The result measured is accurate, reproducible, the specificity of detection and highly sensitive, provides reference for the detection of avilamycin content in edible vegetable oil.
Description
Technical field:
The invention belongs to the detection technique field of edible vegetable oil Pesticides content, relate generally to A Wei in edible vegetable oil
The determination techniques of rhzomorph content.
Background technology:
Avilamycin is the ten hexa-atomic Macrocyclic lactone compounds that a class has parasite killing, mite killing, eelworm-killing activity, to demodicid mite class and
Insecticide has stomach toxicity and action of contace poison, is widely used to poultry, domestic animal endoparasite and ectoparasite and crop pests at present, as posted
Raw blood worm, Diptera, coleoptera, Lepidoptera and pest mite etc..Avilamycin is used for vegetable, melon and fruit, Oryza sativa L., Cotton Gossypii, Brassica campestris L,
After in the various crops such as Chinese crude drug, the insecticide taking food harm in evil demodicid mite and plant tissue there is long residual effect.Owing to having height
Effect, the characteristic of wide spectrum, and side effect is little, good to environment compatibility, avilamycin is favourably welcome in current biological pesticide market
And tool keen competition, the Pest control system of China is occupied more important status.
Edible oil is daily necessities, and common edible oil mostly is Vegetable oil lipoprotein, including Oleum Glycines, Oleum Arachidis hypogaeae semen, rapeseed oil, palm fibre
Palmitic acid oil, olive oil, mustard beggar oil, Oleum Helianthi and Oleum sesami etc., along with economic fast development and people's living standard
Improving constantly, edible vegetable oil consumption figure is in the trend grown steadily, and meanwhile, the safety problem of edible vegetable oil is the most more come
More cause the concern of society.
Research shows, avilamycin belongs to high-toxic pesticide, there is high risk, is the common pesticides of oil crop, and mesh
Front China edible vegetable oil Pesticide Residues detection detection technique has a long way to go, in edible vegetable oil compared with developed countries
The detection research of pesticide residues is the most relatively fewer.Therefore the residual quantity to avilamycin carries out detection and has very important meaning
Justice.Residue analysis method to avilamycin is mainly liquid chromatography at present, and when using UV-detector, sensitivity is the lowest, and
Matrix interference is more serious；And when using fluorescence detector, sensitivity is higher.The residue detection object of avilamycin concentrates on vegetables
In the substrate such as dish, fruit, rice, Folium Camelliae sinensis, the retention analysis report in edible vegetable oil is less.
Summary of the invention:
It is an object of the invention to provide the high-efficiency liquid chromatography method for detecting of avilamycin content in a kind of edible vegetable oil, food
Using ODS C18 Solid-Phase Extraction column purification with vegetable oil sample, HPLC-FLD measures, and result is accurate, reproducible,
The specificity and highly sensitive of detection, when solving use liquid chromatograph-UV-detector, sensitivity is the lowest, and matrix interference is tighter
The technical problem of weight, provides reference for the detection of avilamycin content in edible vegetable oil.
For achieving the above object, the present invention is by the following technical solutions:
In a kind of edible vegetable oil, the high-efficiency liquid chromatography method for detecting of avilamycin content, comprises the steps:
(1) standard working solution is prepared: weigh 0.0200～0.0300g avilamycin standard substance in 100mL volumetric flask,
Dissolve and constant volume with acetonitrile, then by dilution in acetonitrile and be finally configured to 5 standard working solution with Concentraton gradient；
(2) extract sample: weigh 2.00～5.00g food plant oil samples in 50mL tool plug centrifuge tube in, add 10～
After the concussion of 15mL methanol vortex extracts 2～3min, in high speed centrifuge, it is centrifuged 8～10min with 4000～6000r/min, takes
Go out supernatant in 50mL pear shape bottle, add after 10～15mL methanol vortexs concussions extract 1～2min, in high speed centrifuge
It is centrifuged 5～8min with 4000～6000r/min, takes out supernatant, be incorporated in 50mL pear shape bottle, 45 DEG C of water-bath rotary evaporations
After, the sample solution being purified；
(3) sample is purified: with 8～10mL methanol activation ODS C18 solid-phase extraction columns, add in three times with 9～12mL methanol
Enter in the 50mL pear shape bottle described in step (2), after vortex, sample is proceeded in solid-phase extraction column, then with 8～10mL methanol drip washing,
Collection leacheate is in 50mL pear shape bottle, and after 45 DEG C of water-bath rotary evaporations, nitrogen dries up, 2mL acetonitrile constant volume, is taken out 1mL
In 10mL tool plug glass scales test tube, obtain treating the sample solution of derivatization；
(4) analyte derivative: under lucifuge, room temperature environment, adds in the sample treating derivatization prepared by step (3) successively
Enter 0.3～0.5mL N-Methylimidazole. and 0.3～0.5mL trifluoroacetic anhydride, at dark after derivatization 30～40min, toward test tube
In add 1 again～1.5mL methanol, after dark place alcoholization 30～40min, by 0.45 μm membrane filtration, obtain Avermectin to be detected
The sample solution of cellulose content；
(5) prepare substrate and join mark working solution: to blank food plant oil samples by above-mentioned steps (2) and step (3)
After pretreatment mode is extracted and purified, in the pear shape bottle that nitrogen dries up, add the A Wei of gradient concentration prepared by 2mL step (1)
Rhzomorph standard working solution constant volume, is taken out 1mL and fills in glass scales test tube in 10mL tool, use the method pair of step (4)
Sample performs the derivatization, and the substrate of the avilamycin obtaining gradient concentration joins mark working solution；
(6) substrate of the avilamycin of gradient concentration step (5) prepared joins mark working solution and prepared by step (4)
The sample solution of avilamycin content to be detected injects chromatograph of liquid, analyzes after tested and obtains A Wei in food plant oil samples
The content of rhzomorph；
When hplc determination, the chromatographic condition of employing is: chromatographic column: Eclipse XDBC18, wherein chromatographic column
Specification be 5 μm, 4.6 × 150mm；Column temperature: 25 DEG C；Flow velocity: 1mL/min；Sample size: 20 μ L；Flowing phase: the body of methanol/water
Long-pending ratio is 94/6；Excitation wavelength: 365nm, launches wavelength: 470nm.
Preferred as technique scheme, the avilamycin standard work of prepared by step (1) have Concentraton gradient is molten
The concentration of liquid is particularly as follows: 9.393 μ g/mL, 3.7572 μ g/mL, 0.9393 μ g/mL, 0.46965 μ g/mL, 0.18786 μ g/mL.
Preferred as technique scheme, the volume that in step (2), methanol used is extracted in twice vortex concussion is
15mL, the time that concussion is extracted for the first time is 2min, and the time that second time concussion is extracted is 1min, turning of centrifuge used by twice
Speed is 5000r/min, and centrifugation time is 8min.
Preferred as technique scheme, in step (3), used by activation ODS C18 solid-phase extraction column, the volume of methanol is
10mL, in transfer sample to pear shape bottle, the volume of methanol used is 9mL, and the volume of leacheate is 8mL.
Preferred as technique scheme, in step (4), derivatization adds N-Methylimidazole. and the body of trifluoroacetic anhydride
Amassing and be 0.3mL, the time of derivatization is 30min, and it is 1mL that alcoholization methanol used obtains volume, and the alcoholization time is 30min.
The beneficial effects of the present invention is:
1, the reagent that this method uses is less, can effectively extract the avilamycin in edible vegetable oil, cost-effective；
2, pre-treating method is simple, and good purification, it is provided that cleaner upper machine solution decreases instrument and using
Maintenance in journey；
3, result is accurate, reproducible, the specificity of detection and highly sensitive, and recovery of standard addition can reach 92.54%
Above, relative standard deviation (RSD) is below 2.901%；
When 4, solving use liquid chromatograph-UV-detector, sensitivity is the lowest, the technical problem that matrix interference is more serious,
Reference is provided for the detection of avilamycin content in edible vegetable oil.
Detailed description of the invention:
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
Release the present invention, the present invention will not be constituted any restriction.
Embodiment 1
1, instrument and reagent
Chromatograph of liquid Agilent 1100, FLD, Agilent company of the U.S.；
Gas chromatograph Agilent 6890, ECD, Agilent company of the U.S.；
Rotary Evaporators: BUCHI R-210, BUCHI company of Switzerland；
Vortex oscillator: QL-901 type Vortex Haimen City its woods Bel instrument manufacturing company limited；
Nitrogen evaporator: DC-12, Shanghai ANPEL Scientific Instrument Co., Ltd.；
High speed centrifuge: TGL-20B Shanghai City An Ting scientific instrument factory.
Absolute methanol, acetonitrile are chromatographically pure；
Avilamycin standard substance (purity is 93.0%, Dr.Ehrenstorfer GmbH company of Germany).
2, standard working solution is prepared
(1) accurately weigh 0.0202g avilamycin in 100mL volumetric flask, dissolve with acetonitrile and be settled to 100mL,
No. 1 standard reserving solution to 187.86 μ g/mL；
(2) take the mother solution 5mL of above-mentioned numbered 1 in 100mL volumetric flask, be accurately settled to 100mL with acetonitrile, obtain Ah
No. 2 standard reserving solutions that concentration is 9.393 μ g/mL of dimension rhzomorph；
(3) take the mother solution 2mL of above-mentioned numbered 1 in 100mL volumetric flask, be accurately settled to 100mL with acetonitrile, obtain Ah
No. 3 standard reserving solutions that concentration is 3.7572 μ g/mL of dimension rhzomorph；
(4) take the standard reserving solution 5mL of above-mentioned numbered 2 in 50mL volumetric flask, be accurately settled to 50mL with acetonitrile,
Concentration to avilamycin is No. 4 standard reserving solutions of 0.9393 μ g/mL；
(5) take the standard reserving solution 5mL of above-mentioned numbered 2 in 100mL volumetric flask, be accurately settled to 50mL with acetonitrile,
Obtain No. 5 standard reserving solutions that concentration is 0.46965 μ g/mL of avilamycin；
(6) take the standard reserving solution 2mL of above-mentioned numbered 2 in 100mL volumetric flask, be accurately settled to 100mL with acetonitrile
Obtain No. 6 standard reserving solutions that concentration is 0.18786 μ g/mL of avilamycin.
3, sample treatment
Extract: weigh 5.00g food plant oil samples A and fill in centrifuge tube in 50mL tool, add the concussion of 15mL methanol vortex
After extracting 2min, being centrifuged 8min with 5000r/min in high speed centrifuge, taking-up supernatant, in 50mL pear shape bottle, adds
After 1min is extracted in the concussion of 15mL methanol vortex, in high speed centrifuge, it is centrifuged 8min with 5000r/min, takes out supernatant, merge
In 50mL pear shape bottle, 45 DEG C of water-bath rotary evaporations are the most dry, to be clean.
Purify: with 10mL methanol activation ODS C18 solid-phase extraction column (1000mg/6mL), add in three times with 9mL methanol
In above-mentioned 50mL pear shape bottle, after vortex, sample is proceeded in solid-phase extraction column, then with 8mL methanol drip washing, collect leacheate in
In 50mL pear shape bottle, 45 DEG C of water-bath rotary evaporations are the most dry, and nitrogen dries up, 2mL acetonitrile constant volume, are taken out 1mL in 10mL tool plug
In glass scales test tube, treat derivatization.
Analyte derivative: under lucifuge, room temperature environment, in above-mentioned 10mL tool plug glass scales test tube, adds the most respectively
Enter 0.3mL N-Methylimidazole. and 0.3mL trifluoroacetic anhydride, at dark after derivatization 30min, in test tube, add 1mL methanol again,
After refining 30min at Hei An, cross 0.45 μm filter membrane, for the content of the avilamycin in HPLC-FLD detection sample.
4, prepare substrate and join mark working solution
5 blank food plant oil samples are extracted by identical pretreatment mode (with embodiment 1 " 3. sample treatment ")
After purifying, in the pear shape bottle that nitrogen dries up, add the avilamycin standard working solution (embodiment of 2mL variable concentrations gradient
The hybrid standard working solution of " 2. prepare standard working solution " numbering 2-6 in 1) after vortex shakes, it is taken out 1mL in 10mL
In tool plug glass scales test tube, perform the derivatization (processing mode is with " analyte derivative " in embodiment 1 " 3. sample treatment ").
5, assay method
The substrate of the series concentration prepared is joined the sample solution after mark working solution and derivatization and injects liquid chromatograph
Instrument, carries out the quantitative analysis of avilamycin, records after i.e. joining mark working solution sample introduction with the substrate of series concentration with external standard method
After derivatization, the peak area of avilamycin carries out regression analysis to its respective concentration, obtains standard curve；By the sample after derivatization
The peak area that product record after being measured substitutes into standard curve, tries to achieve the content of avilamycin in sample.
When hplc determination, the chromatographic condition of employing is: chromatographic column: Eclipse XDBC18, wherein chromatographic column
Specification be 5 μm, 4.6 × 150mm；Column temperature: 25 DEG C；Flow velocity: 1mL/min；Sample size: 20 μ L；Flowing phase: the body of methanol/water
Long-pending ratio is 94/6；Excitation wavelength: 365nm, launches wavelength: 470nm.
The repeatability of the inventive method and recovery of standard addition experiment:
In blank food plant oil samples, it is separately added into the standard solution of the avilamycin of 3 concentration of 1mL, then divides
By the method for " 3, sample pre-treatments " in embodiment 1, sample is not processed, each concentration do 5 parallel, by embodiment 1
Sample is analyzed by the high-efficient liquid phase chromatogram condition of " 5, assay method ", and calculates it reclaim according to adding scalar sum measured value
Rate, the recovery of standard addition of result avilamycin is between 92.54%～101.65%, and relative standard deviation (RSD) is 1.150%
～between 2.901%, illustrate that the response rate of the inventive method is high, reproducible.
The recovery of standard addition of avilamycin and relative standard deviation in table 1 edible vegetable oil
(n=5)
Embodiment 2:
As described in Example 1, select food plant oil samples B, record the content of avilamycin in sample.
Embodiment 3:
As described in Example 1, select food plant oil samples C, record the content of avilamycin in sample.
Embodiment 4:
As described in Example 1, select food plant oil samples D, record the content of avilamycin in sample.
Embodiment 5:
As described in Example 1, select food plant oil samples E, record the content of avilamycin in sample.
Embodiment 6:
As described in Example 1, select edible vegetable oil sample F, record the content of avilamycin in sample.
In 6 food plant oil samples, the testing result of avilamycin content see table:
The testing result (unit: mg/kg) of avilamycin content in table 2 food plant oil samples
Above-described embodiment is only intended to be illustrated present disclosure rather than limit, therefore with the present invention's
Any change in implication that claims are suitable and scope, is all considered as being included within the scope of the claims.
Claims (10)
1. the high-efficiency liquid chromatography method for detecting of avilamycin content in an edible vegetable oil, it is characterised in that include as follows
Step:
(1) standard working solution is prepared: weigh 0.0200～0.0300g avilamycin standard substance in 100mL volumetric flask, use second
Nitrile dissolves and constant volume, then by dilution in acetonitrile and be finally configured to 5 standard working solution with Concentraton gradient；
(2) sample is extracted: weigh 2.00～5.00g food plant oil samples and fill in centrifuge tube in 50mL tool, add 10～15mL
After the concussion of methanol vortex extracts 2～3min, in high speed centrifuge, it is centrifuged 8～10min with 4000～6000r/min, in taking-up
Clear liquid, in 50mL pear shape bottle, adds 10～15mL methanol vortexs concussions and extracts after 1～2min, in high speed centrifuge with
4000～6000r/min are centrifuged 5～8min, take out supernatant, are incorporated in 50mL pear shape bottle, after 45 DEG C of water-bath rotary evaporations,
The sample solution being purified；
(3) sample is purified: with 8～10mL methanol activation ODS C18 solid-phase extraction columns, add step in three times with 9～12mL methanol
Suddenly in the 50mL pear shape bottle described in (2), after vortex, sample is proceeded in solid-phase extraction column, then with 8～10mL methanol drip washing, collect
Leacheate is in 50mL pear shape bottle, and after 45 DEG C of water-bath rotary evaporations, nitrogen dries up, 2mL acetonitrile constant volume, be taken out 1mL in
In 10mL tool plug glass scales test tube, obtain treating the sample solution of derivatization；
(4) analyte derivative: under lucifuge, room temperature environment, is sequentially added in the sample treating derivatization prepared by step (3)
0.3～0.5mL N-Methylimidazole. and 0.3～0.5mL trifluoroacetic anhydride, at dark after derivatization 30～40min, in test tube
Add 1 again～1.5mL methanol, after refining 30～40min at dark, by 0.45 μm membrane filtration, obtain avilamycin to be detected
The sample solution of content；
(5) prepare substrate and join mark working solution: to blank food plant oil samples by above-mentioned steps (2) and the front place of step (3)
After reason mode is extracted and purified, in the pear shape bottle that nitrogen dries up, add the avilamycin of gradient concentration prepared by 2mL step (1)
Standard working solution constant volume, is taken out 1mL and fills in glass scales test tube in 10mL tool, use the method for step (4) to sample
Performing the derivatization, the substrate of the avilamycin obtaining gradient concentration joins mark working solution；
(6) substrate of the avilamycin of gradient concentration prepared by step (5) join mark working solution and step (4) prepare to be checked
The sample solution surveying avilamycin content injects chromatograph of liquid, analyzes after tested and obtains avilamycin in food plant oil samples
Content；
When hplc determination, the chromatographic condition of employing is: chromatographic column: Eclipse XDBC18, wherein the rule of chromatographic column
Lattice are 5 μm, 4.6 × 150mm；Column temperature: 25 DEG C；Flow velocity: 1mL/min；Sample size: 20 μ L；Flowing phase: the volume ratio of methanol/water
It is 94/6；Excitation wavelength: 365nm, launches wavelength: 470nm.
The high-efficiency liquid chromatography method for detecting of avilamycin content in edible vegetable oil the most according to claim 1, it is special
Levy and be: the concentration of prepared by step (1) the have avilamycin standard working solution of Concentraton gradient is particularly as follows: 9.393 μ g/
mL、3.7572μg/mL、0.9393μg/mL、0.46965μg/mL、0.18786μg/mL。
The high-efficiency liquid chromatography method for detecting of avilamycin content in analysis edible vegetable oil the most according to claim 1,
It is characterized in that: the volume that in step (2), methanol used is extracted in twice vortex concussion is 15mL.
The high-efficiency liquid chromatography method for detecting of avilamycin content in analysis edible vegetable oil the most according to claim 1,
It is characterized in that: the time that vortex concussion for the first time is extracted is 2min, the time that vortex concussion for the second time is extracted is 1min.
The high-efficiency liquid chromatography method for detecting of avilamycin content in analysis edible vegetable oil the most according to claim 1,
It is characterized in that: in step (2), used by twice, the rotating speed of centrifuge is 5000r/min, and centrifugation time is 8min.
The high-efficiency liquid chromatography method for detecting of avilamycin content in edible vegetable oil the most according to claim 1, it is special
Levy and be: in step (3), used by activation ODS C18 solid-phase extraction column, the volume of methanol is 10mL.
The high-efficiency liquid chromatography method for detecting of avilamycin content in edible vegetable oil the most according to claim 1, it is special
Levy and be: in step (3), transfer sample is 9mL to the volume of methanol used in pear shape bottle.
The high-efficiency liquid chromatography method for detecting of avilamycin content in edible vegetable oil the most according to claim 1, it is special
Levy and be: in step (3), the volume of leacheate is 8mL.
The high-efficiency liquid chromatography method for detecting of avilamycin content in edible vegetable oil the most according to claim 1, it is special
Levy and be: in step (4), the volume of derivatization addition N-Methylimidazole. and trifluoroacetic anhydride is 0.3mL, the time of derivatization
For 30min.
The high-efficiency liquid chromatography method for detecting of avilamycin content in edible vegetable oil the most according to claim 1, it is special
Levy and be: in step (4), the volume of alcoholization methanol used is 1mL, and the alcoholization time is 30min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106885853A (en) * | 2017-02-14 | 2017-06-23 | 湖北省农业科学院农业质量标准与检测技术研究所 | The quick pre-treating method for determining AVM pesticide residue in edible oil and quantitative analysis method |
| CN108169390A (en) * | 2017-12-29 | 2018-06-15 | 宁夏希望田野生物农业科技有限公司 | The remaining detection method of avermectin in a kind of bacteria residue |
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