CN106290658B - Avermectin, the quantitative approach of alachlor and procymidone in a kind of edible vegetable oil - Google Patents
Avermectin, the quantitative approach of alachlor and procymidone in a kind of edible vegetable oil Download PDFInfo
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Abstract
The invention discloses avermectin, the quantitative approach of alachlor and procymidone in a kind of edible vegetable oil, it is by sample after methanol is vortexed concussion extraction, with Envi-18 Solid Phase Extraction column purification, sample segment directly analyzes the content of alachlor and procymidone with gas chromatograph, and remaining sample measures the content of avermectin with liquid chromatography-fluorescence with N- methylimidazole and trifluoroacetic anhydride derivatization.The reagent that this method uses is less, can effectively extract avermectin, alachlor and procymidone in edible vegetable oil, save the cost；Sample-pretreating method is simple, provides cleaner upper machine solution, reduces the maintenance of instrument in use；The result of measurement is accurate, reproducible, the specificity and high sensitivity of detection, for detection provides reference while avermectin, alachlor and procymidone content in edible vegetable oil.
Description
Technical field:
The invention belongs to the detection technique field of pesticide concentration in edible vegetable oil, AVM hereinafter in edible vegetable oil is related generally to
The determination techniques of rhzomorph, alachlor and procymidone content.
Background technique:
The 16 of the antibiotics that avermectin is developed first by big village's intelligence of Japanese North university etc. and U.S. Merck company
Membered macrolide compound has efficient, the desinsection of wide spectrum, mite killing, eelworm-killing activity, and mechanism of action and general insecticide are not
Same is interference nervous physiology activity, and stimulation discharges γ-aminobutyric acid, and aminobutyric acid has suppression to the nerve conduction of arthropod
Production is used；Avermectin is widely used to prevention and treatment poultry, epizoa and crop pests in domestic animal body at present, such as parasitic red
Worm, Diptera, coleoptera, Lepidoptera and pest mite etc. are especially used for vegetables, melon and fruit, rice, cotton, rape, Chinese medicine
After in the various crops such as material, the insect endangered feeding in harmful mite and plant tissue has long residual effect, and Small side effects, to ring
Border good compatibility, avermectin are favourably welcome in current biological pesticide market and have keen competition, and the pest in China is anti-
It controls and occupies more important status in system.
Alachlor is soil treatment acetamide-group herbicides before a kind of selective bud, and mechanism of action is by by the children of weeds
Seedling root absorption, interfering nucleic acid and protein synthesis, prevent cell from increasing, to inhibit the growth of root, it is raw then to influence complete stool
It is long, keep weeds dead；Alachlor is preferable to grassy weed effect, can prevent and kill off cotton, corn, rape, peanut, soybean and sugarcane
Middle annual gramineous weed and many broadleaf weeds.
Procymidone is a kind of novel wide spectrum systemic fungicide, the synthesis of triglycerides, tool mainly in inhibition thallus
There are protection and therapeutic effect, using effect is obvious under low temperature, super-humid conditions；Procymidone can be used for rape, radish, eggplant, cucumber,
The crops such as Chinese cabbage, tomato, sunflower, watermelon, strawberry, peach, cherry, flowers, grape, to gray mold, sclerotiniose, grey scab, flower
Maize ear rot, brown rot and blight dis-ease etc. have significant preventive effect, it can also be used to the opportunistic pathogen resistant to thiophanate-methyl, carbendazim.
Edible oil is daily necessities, and common edible oil is mostly vegetable fat, including soya-bean oil, peanut oil, rape seed oil, palm fibre
Palmitic acid oil, olive oil, canola oil, sunflower oil and sesame oil etc. are eaten with the improvement of people ' s living standards and to green
The call of product, while the consumption figure of edible vegetable oil grows steadily, safety problem has also increasingly caused the concern of society.
Studies have shown that avermectin and alachlor belong to high-toxic pesticide, there are high risks, and procymidone then passes through food
Into human body, normal synthesis and metabolism or the inhibition endocrine system of interference human endocrine substance, to the healthy and numerous of the mankind
It grows and also all has a significant impact.Avermectin, alachlor and procymidone are the common pesticides of oil crops, and the edible plant in China at present
Detecting Pesticide detection technique has a long way to go compared with developed countries in object oil, inspection remaining for pesticide in edible vegetable oil
It is also relatively fewer to survey research, therefore detection tool is carried out to the residual quantity of avermectin, alachlor and procymidone in edible vegetable oil
There is very important meaning.It is mainly at present liquid chromatography to the residue analysis method of avermectin, and uses ultraviolet detection
Sensitivity is too low when device, and matrix interference is more serious, and its residue detection object concentrates on the matrix such as veterinary antibiotics, rice, tealeaves
In, the residue analysis method to alachlor and procymidone is mainly gas chromatography, test object be mainly plant sample and
Environmental water sample has not yet to see the retention analysis of avermectin, alachlor and procymidone three simultaneously in edible vegetable oil
Report.
Summary of the invention:
The purpose of the present invention is intended to provide the quantitative square of avermectin in a kind of edible vegetable oil, alachlor and procymidone
Method, food plant oil samples use Envi-18 Solid Phase Extraction column purification, and the content of alachlor and procymidone uses gas chromatography
Measurement, the content of avermectin then uses liquid chromatography-fluorescence to measure, as a result accurately, it is reproducible, the specificity of detection and
High sensitivity, for detection provides reference while avermectin, alachlor and procymidone three's content in edible vegetable oil.
To achieve the above object, the invention adopts the following technical scheme:
Avermectin, the quantitative approach of alachlor and procymidone in a kind of edible vegetable oil, include the following steps:
(1) prepare standard working solution: weighing 0.0500~0.0600g avermectin standard items respectively, 0.0400~
0.0500g alachlor and 0.0400~0.0500g procymidone dissolve simultaneously constant volume in three 100mL volumetric flasks, with acetonitrile, then
With dilution in acetonitrile and finally it is configured to the avermectin with concentration gradient, the hybrid standard of three kinds of pesticides of alachlor and procymidone
Working solution；
(2) it extracts sample: weighing 5.00g food plant oil samples and have in plug centrifuge tube in 50mL, 15mL methanol whirlpool is added
After 2min is extracted in rotation concussion, 10min is centrifuged with 6000r/min in supercentrifuge, takes out supernatant in 50mL pear shape bottle,
It adds 10mL methanol to be vortexed after concussion extraction 1min, 6min is centrifuged with 6000r/min in supercentrifuge, takes out supernatant
Liquid is incorporated in 50mL pear shape bottle, after 45 DEG C of water-bath rotary evaporations, obtains sample to be clean；
(3) it purifies sample: activating Envi-18 solid-phase extraction column with 10mL methanol, step is added in three times with 12mL methanol
(2) in the 50mL pear shape bottle described in, sample is transferred in solid-phase extraction column after vortex, then is eluted with 10mL methanol, elution is collected
Liquid after 45 DEG C of water-bath rotary evaporations, is dried with nitrogen in 50mL pear shape bottle, 2mL acetonitrile constant volume, is taken out 1mL and has in 10mL
It fills in glass scales test tube, obtains the sample to derivatization；Remaining sample solution is obtained to be checked by 0.45 μm of membrane filtration
Survey the sample solution of alachlor and two kinds of pesticide concentrations of procymidone；
(4) sample derivatization: being protected from light, under room temperature environment, and the sample to derivatization prepared by step (3) is sequentially added
0.3mL N- methylimidazole and 0.3mL trifluoroacetic anhydride, dark place derivatization 40min after, into test tube again add 1mL methanol, it is black
After 40min is refined in dark place, 0.45 μm of filter membrane is crossed, the sample solution of avermectin content to be detected is obtained；
(5) prepare matrix with mark working solution: identical by step (2) and step (3) to blank food plant oil samples
After pretreatment mode is extracted and purified, the AVM hereinafter of the gradient concentration of 2mL step (1) preparation is added in the pear shape bottle being dried with nitrogen
The hybrid standard working solution of three kinds of rhzomorph, alachlor and procymidone pesticides is vortexed after concussion, is taken out 1mL and has in 10mL
It fills in glass scales test tube, is performed the derivatization by the method for step (4), obtain avermectin, alachlor and the corruption of gradient concentration
The matrix of mould sharp three kinds of pesticides is with mark working solution；
(6) avermectin of the gradient concentration of step (1) preparation, the work of the standard of three kinds of pesticides of alachlor and procymidone are molten
The sample solution of the alachlor to be detected and two kinds of pesticide concentrations of procymidone of liquid and step (3) preparation injects gas chromatograph, warp
Test analysis obtains the content of alachlor and procymidone in food plant oil samples；
By the avermectin of the gradient concentration of step (5) preparation, the matrix of three kinds of pesticides of alachlor and procymidone with mark work
The sample solution injection liquid chromatograph for making the avermectin content to be detected of solution and step (4) preparation, is analyzed after tested
The content of avermectin into food plant oil samples.
As a preferred embodiment of the above technical solution, the test condition of gas chromatograph described in step (6) are as follows: chromatographic column: HP-
5, wherein the specification of chromatographic column is 30m × 0.2mm × 0.33 μm；Injector temperature: 260 DEG C；Sample introduction mode: it does not shunt；Sample introduction
Amount: 2 μ L；Detector temperature: 290 DEG C；Column initial temperature is 80 DEG C, 200 DEG C is warming up to 20 DEG C/min rate, with 5 DEG C/min
Rate is warming up to 250 DEG C, is warming up to 280 DEG C with 10 DEG C/min rate, keeps 5min.
As a preferred embodiment of the above technical solution, the test condition of gas chromatograph described in step (6) are as follows: chromatographic column:
Eclipse XDB C18, wherein the specification of chromatographic column is 5 μm, 4.6 × 150mm；Column temperature: 25 DEG C；Flow velocity: 1mL/min；Sample introduction
Amount: 20 μ L；Mobile phase: the volume ratio of methanol/water is 94/6；Excitation wavelength: 365nm, launch wavelength: 470nm.
As a preferred embodiment of the above technical solution, three kinds of avermectin with concentration gradient, alachlor and procymidone pesticides
Hybrid standard working solution preparation method it is as follows:
(1) it accurately weighs 0.0512g avermectin to be dissolved in 100mL volumetric flask with acetonitrile, and is accurately settled to
100mL obtains the avermectin standard reserving solution of 476.16 μ g/mL；
(2) it accurately weighs 0.0431g alachlor to be dissolved in 100mL volumetric flask with acetonitrile, and is accurately settled to 100mL,
Obtain the alachlor standard reserving solution of 420.225 μ g/mL；
(3) it accurately weighs 0.0433g procymidone to be dissolved in 100mL volumetric flask with acetonitrile, and is accurately settled to 100mL,
Obtain the procymidone standard reserving solution of 430.835 μ g/mL；
(4) the alachlor mark of the avermectin standard reserving solution, 5mL step (2) preparation that take 5mL step (1) to prepare respectively
Quasi- stock solution and the procymidone standard reserving solution of 5mL step (3) preparation are accurately settled in 50mL volumetric flask with acetonitrile
50mL, obtain avermectin, alachlor, procymidone concentration be followed successively by 47.616 μ g/mL, 42.0225 μ g/mL, 43.0835 μ
The standard reserving solution of g/mL；
(5) the alachlor mark of the avermectin standard reserving solution, 2mL step (2) preparation that take 2mL step (1) to prepare respectively
Quasi- stock solution and the procymidone standard reserving solution of 2mL step (3) preparation are accurately settled in 100mL volumetric flask with acetonitrile
100mL, obtain avermectin, alachlor, procymidone concentration be followed successively by 9.5232 μ g/mL, 8.4045 μ g/mL, 8.6167 μ g/
The standard reserving solution of mL；
(6) the standard reserving solution 5mL for taking step (4) to prepare accurately is settled to 100mL with acetonitrile in 100mL volumetric flask,
Obtain avermectin, alachlor, procymidone concentration be followed successively by 2.3808 μ g/mL, 2.101125 μ g/mL, 2.154175 μ g/mL
Standard reserving solution；
(7) the standard reserving solution 2mL for taking step (4) to prepare accurately is settled to 100mL with acetonitrile in 100mL volumetric flask,
Obtain avermectin, alachlor, procymidone concentration be followed successively by 0.95232 μ g/mL, 0.84045 μ g/mL, 0.86167 μ g/mL
Standard reserving solution；
(8) the standard reserving solution 5mL for taking step (5) to prepare accurately is settled to 100mL with acetonitrile in 100mL volumetric flask,
Obtain avermectin, alachlor, procymidone concentration be followed successively by 0.47616 μ g/mL, 0.420225 μ g/mL, 0.430835 μ g/
The standard reserving solution of mL；
(9) the standard reserving solution 5mL for taking step (6) to prepare accurately is settled to 50mL with acetonitrile, obtains in 50mL volumetric flask
Concentration to avermectin, alachlor, procymidone is followed successively by 0.23808 μ g/mL, 0.2101125 μ g/mL, 0.2154175 μ g/
The standard reserving solution of mL；
(10) the standard reserving solution 5mL for taking step (6) to prepare accurately is settled to 100mL with acetonitrile in 100mL volumetric flask
Obtain avermectin, alachlor, procymidone concentration be followed successively by 0.11904 μ g/mL, 0.10505625 μ g/mL, 0.10770875
The standard reserving solution of μ g/mL.
The beneficial effects of the present invention are:
1, the reagent that this method uses is less, and it is mould effectively to extract avermectin in edible vegetable oil, alachlor and corruption
Benefit, save the cost.
2, pre-treating method is simple, good purification, provides cleaner upper machine solution, reduces instrument and using
Maintenance in journey.
3, result is accurate, reproducible, and the specificity and high sensitivity of detection, the average recovery rate of method is 91.72%
Between~95.75%, relative standard deviation (RSD) is between 1.708%~4.297%.
4, it when measuring the content of avermectin in edible vegetable oil, solves using clever when liquid chromatogram-UV detector
Sensitivity is too low, the more serious technical problem of matrix interference.
Specific embodiment:
Embodiment 1
1. instrument and reagent
Liquid chromatograph 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: its woods Bell's instrument manufacturing Co., Ltd of the Haimen City QL-901 type Vortex；
Nitrogen evaporator: DC-12, Shanghai ANPEL Scientific Instrument Co., Ltd.；
Supercentrifuge: the Shanghai City TGL-20B An Ting scientific instrument factory.
Anhydrous methanol, acetonitrile are chromatographically pure；
Avermectin standard items (purity 93.0%, German Dr.Ehrenstorfer GmbH company)；
Alachlor standard items (purity 97.5%, German Dr.Ehrenstorfer GmbH company)；
Procymidone standard items (purity 99.5%, German Dr.Ehrenstorfer GmbH company).
2. preparing standard working solution
(1) it accurately weighs 0.0512g avermectin to be dissolved in 100mL volumetric flask with acetonitrile, and is accurately settled to
100mL obtains No. 1 standard reserving solution of 476.16 μ g/mL；
(2) it accurately weighs 0.0431g alachlor to be dissolved in 100mL volumetric flask with acetonitrile, and is accurately settled to 100mL
Obtain No. 2 standard reserving solutions of 420.225 μ g/mL；
(3) it accurately weighs 0.0433g procymidone to be dissolved in 100mL volumetric flask with acetonitrile, and is accurately settled to 100mL
Obtain No. 3 standard reserving solutions of 430.835 μ g/mL；
(4) it takes three kinds of each 5mL of mother liquor of above-mentioned number 1-3 in 50mL volumetric flask respectively, is accurately settled to acetonitrile
50mL obtain avermectin, alachlor, procymidone concentration be followed successively by 47.616 μ g/mL, 42.0225 μ g/mL, 43.0835 μ g/
No. 4 standard reserving solutions of mL；
(5) take three kinds of each 2mL of mother liquor of above-mentioned number 1-3 in 100mL volumetric flask respectively, with the accurate constant volume of acetonitrile
To 100mL obtain avermectin, alachlor, procymidone concentration be followed successively by 9.5232 μ g/mL, 8.4045 μ g/mL, 8.6167 μ
No. 5 standard reserving solutions of g/mL；
(6) it takes the standard reserving solution 5mL that above-mentioned number is 4 in 100mL volumetric flask, is accurately settled to 100mL with acetonitrile
Obtain avermectin, alachlor, procymidone concentration be followed successively by 2.3808 μ g/mL, 2.101125 μ g/mL, 2.154175 μ g/mL
No. 6 standard reserving solutions；
(7) it takes the standard reserving solution 2mL that above-mentioned number is 4 in 100mL volumetric flask, is accurately settled to 100mL with acetonitrile
Obtain avermectin, alachlor, procymidone concentration be followed successively by 0.95232 μ g/mL, 0.84045 μ g/mL, 0.86167 μ g/mL
No. 7 standard reserving solutions；
(8) it takes the standard reserving solution 5mL that above-mentioned number is 5 in 100mL volumetric flask, is accurately settled to 100mL with acetonitrile
Obtain avermectin, alachlor, procymidone concentration be followed successively by 0.47616 μ g/mL, 0.420225 μ g/mL, 0.430835 μ g/
No. 8 standard reserving solutions of mL；
(9) it takes the standard reserving solution 5mL that above-mentioned number is 6 in 50mL volumetric flask, 50mL is accurately settled to acetonitrile and is obtained
Concentration to avermectin, alachlor, procymidone is followed successively by 0.23808 μ g/mL, 0.2101125 μ g/mL, 0.2154175 μ g/
No. 9 standard reserving solutions of mL；
(10) it takes the standard reserving solution 5mL that above-mentioned number is 6 in 100mL volumetric flask, is accurately settled to 100mL with acetonitrile
Obtain avermectin, alachlor, procymidone concentration be followed successively by 0.11904 μ g/mL, 0.10505625 μ g/mL, 0.10770875
No. 10 standard reserving solutions of μ g/mL.
3. sample treatment
It extracts sample: weighing 5.00g food plant oil samples and have in plug centrifuge tube in 50mL, the vortex shake of 15mL methanol is added
It swings after extracting 2min, 10min is centrifuged with 6000r/min in supercentrifuge, take out supernatant in 50mL pear shape bottle, then plus
Enter 10mL methanol to be vortexed after concussion extraction 1min, 6min is centrifuged with 6000r/min in supercentrifuge, takes out supernatant, is closed
And in 50mL pear shape bottle, 45 DEG C of water-bath rotary evaporations are closely dry, to be clean.
It purifies sample: activating Envi-18 solid-phase extraction column (1000mg/6mL) with 10mL methanol, in three times with 12mL methanol
It is added in above-mentioned 50mL pear shape bottle, sample is transferred in solid-phase extraction column after vortex, then eluted with 10mL methanol, collect leacheate
In 50mL pear shape bottle, 45 DEG C of water-bath rotary evaporations are closely dry, are dried with nitrogen, 2mL acetonitrile constant volume, are taken out 1mL and have in 10mL
It fills in glass scales test tube, to derivatization；Remaining sample solution crosses 0.45 μm of filter membrane, in gas-chromatography difference test sample
Alachlor and two kinds of pesticides of procymidone content.
Sample derivatization: being protected from light, under room temperature environment, has in plug glass scales test tube in above-mentioned 10mL and is successively separately added into
0.3mL N- methylimidazole and 0.3mL trifluoroacetic anhydride, dark place derivatization 40min after, into test tube again add 1mL methanol, it is black
After 40min is refined in dark place, 0.45 μm of filter membrane is crossed, for the content of the avermectin in HPLC-FLD test sample.
4. preparing matrix with mark working solution
6 blank food plant oil samples are extracted by embodiment 1 " 3. sample treatment " identical pretreatment mode and net
After change, respectively at avermectin, the first that the various concentration of number 5-10 in 2mL embodiment 1 is added in the pear shape bottle being dried with nitrogen
The hybrid standard working solution of three kinds of pesticides of careless amine and procymidone is vortexed after concussion, is taken out 1mL in 10mL and has plug glass quarter
It spends in test tube, is performed the derivatization by " sample derivatization " identical processing mode in embodiment 1 " 3. sample treatment ".
5. measuring method
(1) measuring method of alachlor and procymidone residual quantity: by the standard working solution of prepared series of concentrations and
The sample solution of underivatized injects gas chromatograph, the quantitative analysis of alachlor and procymidone is carried out with external standard method, i.e., with gas
The peak area of alachlor and procymidone carries out regression analysis to its respective concentration respectively after analysis of hplc, obtains standard curve；
Will sample carry out gas Chromatographic Determination after the peak area that measures substitute into standard curve, acquire containing for alachlor and procymidone in sample
Amount.
In gas chromatograph for determination, the chromatographic condition of use are as follows: (wherein the specification of chromatographic column is 30m × 0.2mm to HP-5
×0.33μm)；Injector temperature: 260 DEG C；Sample introduction mode: it does not shunt；Sample volume: 2 μ L；Detector temperature: 290 DEG C；Column is initial
Temperature is 80 DEG C, is warming up to 200 DEG C with 20 DEG C/min rate, 250 DEG C is warming up to 5 DEG C/min rate, with 10 DEG C/min rate
280 DEG C are warming up to, 5min is kept.
(2) measuring method of Determination of Abamectin Residue: the matrix of prepared series of concentrations with mark working solution and is spread out
Sample solution after biochemistry injects liquid chromatograph, the quantitative analysis of avermectin is carried out with external standard method, i.e., with series of concentrations
Matrix carries out regression analysis to its respective concentration with the peak area of avermectin after the derivatization measured after mark working solution sample introduction,
Obtain standard curve；The peak area that measures after sample after derivatization is measured substitutes into standard curve, acquire in sample Ah
Tie up the content of rhzomorph.
In hplc determination, the chromatographic condition of use are as follows: chromatographic column: Eclipse XDB C18 (wherein chromatographic column
Specification be 5 μm, 4.6 × 150mm)；Column temperature: 25 DEG C；Flow velocity: 1mL/min；Sample volume: 20 μ L；Mobile phase: the body of methanol/water
Product is than being 94/6；Excitation wavelength: 365nm, launch wavelength: 470nm.
Repeatability and the recovery of standard addition experiment of the method for the present invention:
The avermectin of 3 concentration of 1mL, alachlor and procymidone are separately added into blank food plant oil samples
Then mixed standard solution is respectively handled sample by the method for " 3, sample pre-treatments " in embodiment 1, each concentration is done
5 parallel, analyzes by the high-efficient liquid phase chromatogram condition of " 5, measuring method " in embodiment 1 sample, and according to scalar quantity
Its rate of recovery is calculated with measured value, as a result the recovery of standard addition of avermectin is between 91.22%~101.3%, relative standard
Deviation (RSD) is between 1.708%~3.937%, and the recovery of standard addition of alachlor is between 89.26%~100.3%, relatively
Standard deviation (RSD) between 2.480%~4.297%, the recovery of standard addition of procymidone between 88.32%~100.1%,
Relative standard deviation (RSD) illustrates that the rate of recovery of the method for the present invention is high between 2.983%~3.167%, reproducible.
Avermectin, the recovery of standard addition of alachlor and procymidone and relative standard deviation (n=in 1 edible vegetable oil of table
5)
Embodiment 2:
As described in Example 1, food plant oil samples B is selected, avermectin in sample, alachlor and procymidone are measured
Content.
Embodiment 3:
As described in Example 1, food plant oil samples C is selected, avermectin in sample, alachlor and procymidone are measured
Content.
Embodiment 4:
As described in Example 1, food plant oil samples D is selected, avermectin in sample, alachlor and procymidone are measured
Content.
Embodiment 5:
As described in Example 1, food plant oil samples E is selected, avermectin in sample, alachlor and procymidone are measured
Content.
Embodiment 6:
As described in Example 1, edible vegetable oil sample F is selected, avermectin in sample, alachlor and procymidone are measured
Content.
Avermectin in 6 food plant oil samples, alachlor and procymidone content test results in the following table:
The testing result (unit: mg/kg) of avermectin, alachlor and procymidone content in 2 food plant oil samples of table
The above embodiments are merely intended to illustrate the present invention rather than to limit it, thus with it is of the invention
Any change in the comparable meaning and scope of claims, should be construed as being included in the scope of the claims.
Claims (1)
1. avermectin, the quantitative approach of alachlor and procymidone in a kind of edible vegetable oil, which is characterized in that including walking as follows
It is rapid:
(1) prepare standard working solution: weighing 0.0500~0.0600g avermectin standard items, 0.0400~0.0500g respectively
Alachlor and 0.0400~0.0500g procymidone, with acetonitrile dissolution and constant volume, then use acetonitrile in three 100mL volumetric flasks
Dilute and be finally configured to have the avermectin of concentration gradient, three kinds of pesticides of alachlor and procymidone hybrid standard work it is molten
Liquid；
(2) it extracts sample: weighing 5.00g food plant oil samples and have in plug centrifuge tube in 50mL, the vortex shake of 15mL methanol is added
It swings after extracting 2min, 10min is centrifuged with 6000r/min in supercentrifuge, take out supernatant in 50mL pear shape bottle, then plus
Enter 10mL methanol to be vortexed after concussion extraction 1min, 6min is centrifuged with 6000r/min in supercentrifuge, takes out supernatant, is closed
And in 50mL pear shape bottle, after 45 DEG C of water-bath rotary evaporations, sample to be clean is obtained；
(3) it purifies sample: activating Envi-18 solid-phase extraction column with 10mL methanol, step (2) institute is added in three times with 12mL methanol
In the 50mL pear shape bottle stated, sample is transferred in solid-phase extraction column after vortex, then with 10mL methanol elute, collect leacheate in
It in 50mL pear shape bottle, after 45 DEG C of water-bath rotary evaporations, is dried with nitrogen, 2mL acetonitrile constant volume, is taken out 1mL in 10mL and has plug glass
In glass scale test tube, the sample to derivatization is obtained；Remaining sample solution obtains first to be detected by 0.45 μm of membrane filtration
The sample solution of careless amine and two kinds of pesticide concentrations of procymidone；
(4) sample derivatization: being protected from light, under room temperature environment, and the sample to derivatization prepared by step (3) is sequentially added
0.3mL N- methylimidazole and 0.3mL trifluoroacetic anhydride, dark place derivatization 40min after, into test tube again add 1mL methanol, it is black
After 40min is refined in dark place, 0.45 μm of filter membrane is crossed, the sample solution of avermectin content to be detected is obtained；
(5) prepare matrix with mark working solution: to blank food plant oil samples by step (2) and step (3) extraction and purification
Afterwards, the avermectin with concentration gradient, alachlor and the corruption of 2mL step (1) preparation are added in the pear shape bottle being dried with nitrogen
The hybrid standard working solution of mould sharp three kinds of pesticides is vortexed after concussion, is taken out 1mL in 10mL and has plug glass scales test tube
In, it is performed the derivatization by the method for step (4), obtains that there is three kinds of avermectin of concentration gradient, alachlor and procymidone agricultures
The matrix of medicine is with mark working solution；
(6) avermectin with concentration gradient of step (1) preparation, the work of the standard of three kinds of pesticides of alachlor and procymidone are molten
The sample solution of the alachlor to be detected and two kinds of pesticide concentrations of procymidone of liquid and step (3) preparation injects gas chromatograph, warp
Test analysis obtains the content of alachlor and procymidone in food plant oil samples；
By the avermectin with concentration gradient of step (5) preparation, the matrix of three kinds of pesticides of alachlor and procymidone with mark work
The sample solution injection liquid chromatograph for making the avermectin content to be detected of solution and step (4) preparation, is analyzed after tested
The content of avermectin into food plant oil samples；
The test condition of gas chromatograph described in step (6) are as follows: chromatographic column: HP-5, wherein the specification of chromatographic column be 30m ×
0.2mm×0.33μm；Injector temperature: 260 DEG C；Sample introduction mode: it does not shunt；Sample volume: 2 μ L；Detector temperature: 290 DEG C；Column
Initial temperature is 80 DEG C, is warming up to 200 DEG C with 20 DEG C/min rate, is then warming up to 250 DEG C with 5 DEG C/min rate, then with 10
DEG C/min rate is warming up to 280 DEG C, keep 5min；
The test condition of liquid chromatograph described in step (6) are as follows: chromatographic column: Eclipse XDBC18, wherein rule of chromatographic column
Lattice are 5 μm, 4.6 × 150mm；Column temperature: 25 DEG C；Flow velocity: 1mL/min；Sample volume: 20 μ L；Mobile phase: the volume ratio of methanol/water
It is 94/6；Excitation wavelength: 365nm, launch wavelength: 470nm；
With three kinds of avermectin of concentration gradient, alachlor and procymidone pesticides described in step (1), (5) or (6)
The preparation method of hybrid standard working solution is as follows:
(1) it accurately weighs 0.0512g avermectin to be dissolved in 100mL volumetric flask with acetonitrile, and is accurately settled to 100mL, obtain
To the avermectin standard reserving solution of 476.16 μ g/mL；
(2) it accurately weighs 0.0431g alachlor to be dissolved in 100mL volumetric flask with acetonitrile, and is accurately settled to 100mL, obtain
420.225 the alachlor standard reserving solution of μ g/mL；
(3) it accurately weighs 0.0433g procymidone to be dissolved in 100mL volumetric flask with acetonitrile, and is accurately settled to 100mL, obtain
430.835 the procymidone standard reserving solution of μ g/mL；
(4) the alachlor standard storage of the avermectin standard reserving solution, 5mL step (2) preparation that take 5mL step (1) to prepare respectively
Procymidone standard reserving solution prepared by standby liquid and 5mL step (3) is accurately settled to 50mL with acetonitrile, obtains in 50mL volumetric flask
Concentration to avermectin, alachlor, procymidone is followed successively by the mark of 47.616 μ g/mL, 42.0225 μ g/mL, 43.0835 μ g/mL
Quasi- stock solution；
(5) the alachlor standard storage of the avermectin standard reserving solution, 2mL step (2) preparation that take 2mL step (1) to prepare respectively
Procymidone standard reserving solution prepared by standby liquid and 2mL step (3) is accurately settled to 100mL with acetonitrile in 100mL volumetric flask,
Obtain avermectin, alachlor, procymidone concentration be followed successively by the mark of 9.5232 μ g/mL, 8.4045 μ g/mL, 8.6167 μ g/mL
Quasi- stock solution；
(6) the standard reserving solution 5mL for taking step (4) to prepare accurately is settled to 100mL with acetonitrile, obtains in 100mL volumetric flask
Avermectin, alachlor, procymidone concentration be followed successively by the mark of 2.3808 μ g/mL, 2.101125 μ g/mL, 2.154175 μ g/mL
Quasi- stock solution；
(7) the standard reserving solution 2mL for taking step (4) to prepare accurately is settled to 100mL with acetonitrile, obtains in 100mL volumetric flask
Avermectin, alachlor, procymidone concentration be followed successively by the mark of 0.95232 μ g/mL, 0.84045 μ g/mL, 0.86167 μ g/mL
Quasi- stock solution；
(8) the standard reserving solution 5mL for taking step (5) to prepare accurately is settled to 100mL with acetonitrile, obtains in 100mL volumetric flask
Avermectin, alachlor, procymidone concentration be followed successively by 0.47616 μ g/mL, 0.420225 μ g/mL, 0.430835 μ g/mL
Standard reserving solution；
(9) take step (6) prepare standard reserving solution 5mL in 50mL volumetric flask, be accurately settled to 50mL with acetonitrile, obtain Ah
Dimension rhzomorph, alachlor, procymidone concentration be followed successively by 0.23808 μ g/mL, 0.2101125 μ g/mL, 0.2154175 μ g/mL
Standard reserving solution；
(10) the standard reserving solution 5mL for taking step (6) to prepare accurately is settled to 100mL with acetonitrile and obtains in 100mL volumetric flask
Avermectin, alachlor, procymidone concentration be followed successively by 0.11904 μ g/mL, 0.10505625 μ g/mL, 0.10770875 μ g/
The standard reserving solution of mL.
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