CN115406993B - HLPC method for detecting 2-methyl-4-chloroisooctyl ester and fluroxypyr-meptyl acetate - Google Patents
HLPC method for detecting 2-methyl-4-chloroisooctyl ester and fluroxypyr-meptyl acetate Download PDFInfo
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- CN115406993B CN115406993B CN202211063617.9A CN202211063617A CN115406993B CN 115406993 B CN115406993 B CN 115406993B CN 202211063617 A CN202211063617 A CN 202211063617A CN 115406993 B CN115406993 B CN 115406993B
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- -1 2-methyl-4-chloroisooctyl ester Chemical class 0.000 title claims abstract description 93
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000012488 sample solution Substances 0.000 claims abstract description 35
- 239000005558 Fluroxypyr Substances 0.000 claims abstract description 26
- 238000001514 detection method Methods 0.000 claims abstract description 22
- OLZQTUCTGLHFTQ-UHFFFAOYSA-N octan-2-yl 2-(4-amino-3,5-dichloro-6-fluoropyridin-2-yl)oxyacetate Chemical group CCCCCCC(C)OC(=O)COC1=NC(F)=C(Cl)C(N)=C1Cl OLZQTUCTGLHFTQ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000523 sample Substances 0.000 claims description 46
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 33
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 239000012086 standard solution Substances 0.000 claims description 12
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 9
- 229940050176 methyl chloride Drugs 0.000 claims description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
- 239000004548 suspo-emulsion Substances 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 239000000575 pesticide Substances 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 abstract 1
- FGDQGIKMWOAFIK-UHFFFAOYSA-N acetonitrile;phosphoric acid Chemical compound CC#N.OP(O)(O)=O FGDQGIKMWOAFIK-UHFFFAOYSA-N 0.000 abstract 1
- 230000014759 maintenance of location Effects 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 239000012071 phase Substances 0.000 description 8
- 241000196324 Embryophyta Species 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 239000000725 suspension Substances 0.000 description 6
- MEFQWPUMEMWTJP-UHFFFAOYSA-N fluroxypyr Chemical compound NC1=C(Cl)C(F)=NC(OCC(O)=O)=C1Cl MEFQWPUMEMWTJP-UHFFFAOYSA-N 0.000 description 5
- SFGBOBMTMFHZJH-UHFFFAOYSA-N 1-chloro-6-methylheptane Chemical compound CC(C)CCCCCCl SFGBOBMTMFHZJH-UHFFFAOYSA-N 0.000 description 4
- 238000003556 assay Methods 0.000 description 4
- 239000004009 herbicide Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000010812 external standard method Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000002363 herbicidal effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 241000209140 Triticum Species 0.000 description 2
- 235000021307 Triticum Nutrition 0.000 description 2
- 240000008042 Zea mays Species 0.000 description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 2
- 235000005822 corn Nutrition 0.000 description 2
- 229940088597 hormone Drugs 0.000 description 2
- 239000005556 hormone Substances 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
- 238000004007 reversed phase HPLC Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000009885 systemic effect Effects 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 240000005979 Hordeum vulgare Species 0.000 description 1
- 235000007340 Hordeum vulgare Nutrition 0.000 description 1
- DICUPLXUNISGAQ-UHFFFAOYSA-N Isooctyl acetate Chemical compound CC(C)CCCCCOC(C)=O DICUPLXUNISGAQ-UHFFFAOYSA-N 0.000 description 1
- 240000001140 Mimosa pudica Species 0.000 description 1
- 235000016462 Mimosa pudica Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 241000329195 Sparganium erectum Species 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 239000002420 orchard Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Classifications
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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
-
- 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
-
- 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
- G01N30/74—Optical detectors
-
- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention belongs to the technical field of pesticide detection, and provides an HLPC method for detecting 2 methyl 4-chloroisooctyl and fluroxypyr isooctyl: and (3) taking a C18 column as a chromatographic column, taking an acetonitrile-phosphoric acid aqueous solution with the pH of 3-3.5 as a mobile phase, detecting an ultraviolet absorption value at 235nm, and calculating the mass fraction of 2 methyl 4 chloroisooctyl ester or fluroxypyr meptyl in the sample solution to be detected according to the peak area. The invention can finish the simultaneous detection of the 2-methyl-4-chloroisooctyl ester and the fluroxypyr-meptyl ester under the same chromatographic condition, has good separation effect and short peak-to-peak time, and improves the detection efficiency while ensuring the accuracy.
Description
Technical Field
The invention belongs to the technical field of pesticide detection, and particularly relates to an HLPC method for detecting 2-methyl-4-chloroisooctyl ester and fluroxypyr-meptyl.
Background
The 2-methyl-4-chloroisooctyl ester is a selective systemic hormone herbicide, can destroy the transmission tissue of dicotyledonous plants, and is mainly used for preventing and killing annual and perennial broadleaf weeds and common burreed herb of crops such as rice, wheat, corn and the like. The fluroxypyr is a systemic conduction type post-emergence stem and leaf herbicide, which is absorbed by weeds quickly after application, so that sensitive plants react with typical hormone herbicides and are conducted to all parts of the whole plant, the plant is deformed and distorted, and finally dies. Is suitable for preventing and killing broadleaf weeds in wheat, barley, corn, grape, orchard, pasture, woodland, lawn and other fields. The two components are combined, and the binary compound herbicide taking 2-methyl-4-chloroisooctyl and fluroxypyr as active ingredients is newly introduced in recent years, and is popular in the market due to the advantages of high efficiency, rapidness and wide application range of crops. The product is prepared by compounding two effective components, and in the quality detection of the product, the two effective components are required to be detected, if the two effective components can be detected simultaneously under the same chromatographic condition, the detection time can be greatly saved, the detection cost can be reduced, and the detection efficiency can be improved.
At present, a HPLC method is used for detecting 2-methyl-4-chloroisooctyl ester, a methanol is adopted to dissolve a sample, a methanol+phosphoric acid aqueous solution (pH 4) is used as a mobile phase, a stainless steel column with C18 as a filler and a variable wavelength ultraviolet detector are used, and reversed-phase high performance liquid chromatography separation and determination and external standard method quantification are carried out on the 2-methyl-4-chloroisooctyl ester in the sample; however, under this condition, the impurities of the fluroxypyr-meptyl can not be completely separated, the accuracy is low, and the detection error is large. In the HPLC detection of the fluroxypyr-meptyl, a sample is dissolved by a mobile phase, acetonitrile-water is used as the mobile phase, and a C18 column and an ultraviolet detector are used for high performance liquid chromatography separation and determination of the fluroxypyr-meptyl in the sample, and the external standard method is used for quantification. When the method is used for detection, the peak time of the 2-methyl-4-chloroisooctyl ester is long, and the detection time is long.
Disclosure of Invention
Aiming at the problem of lack of a high-efficiency liquid phase detection method for simultaneously detecting 2-methyl-4-chloroisooctyl ester and fluroxypyr-meptyl, the invention provides an HLPC method for simultaneously detecting 2-methyl-4-chloroisooctyl ester and fluroxypyr-meptyl, which can simultaneously detect two effective components under the same chromatographic condition, has good separation effect, ensures accuracy and improves detection efficiency.
In order to achieve the above purpose, the present invention adopts the following technical scheme.
An HLPC method for detecting isooctyl 2-methyl-4-chloride and isooctyl fluroxypyr, comprising the steps of:
(1) Preparing a standard solution of 2 methyl 4-chloroisooctyl-fluroxypyr-meptyl;
(2) Obtaining a sample solution to be tested;
(3) The peak areas of the 2-methyl-4-chloroisooctyl-fluroxypyr standard solution and the sample solution to be tested are respectively measured under the following high performance liquid chromatography conditions:
chromatographic column: a C18 column, which is provided with a plurality of holes,
mobile phase: acetonitrile-pH 3-3.5 phosphoric acid solution with the volume ratio of 80:20-85:15,
flow rate: 0.8-1.5mL/min,
column temperature: 25-35 ℃,
detection wavelength: at a wavelength of 235nm,
sample injection volume: 5-10 mu L;
(4) And calculating the mass fraction of the 2-methyl-4-chloroisooctyl ester or the chlorofluopicolide isooctyl acetate in the sample solution to be detected.
Preferably, in the step (2), the obtaining step of the sample solution to be measured is: samples of the formulations containing isooctyl 2-methyl-4-chloro and/or isooctyl fluroxypyr-meptyl are extracted and diluted with a suitable solvent. More preferably, the solvent of extraction is acetonitrile.
Preferably, in step (3), the packing particle size of the column is 3-5 μm, the length of the column is 150-250mm, and the inner diameter is 2-4.6mm.
Preferably, in the step (4), the mass fraction X of the 2-methyl-4-chloroisooctyl ester or the fluroxypyr-meptyl ester in the sample solution to be tested is calculated according to the following formula 1 ：
X 1 =
Wherein:
A 1 peak area of 2 methyl 4 chloroisooctyl ester or fluroxypyr-meptyl in the standard solution;
A 2 peak area of 2 methyl 4 chloroisooctyl ester or fluroxypyr-meptyl in sample solution;
m 1 -2 methyl 4 chloroisooctyl ester or fluroxypyr-meptyl ester) standard mass, g;
m 2 sample mass，g；
The mass fraction of the 2-methyl-4-chloroisooctyl ester or the chlorofluopicolide in the P-standard sample is percent.
The invention has the following advantages:
the invention uses acid acetonitrile as mobile phase, uses C18 column and ultraviolet detector with variable wavelength to separate and measure 2 methyl 4 isooctyl chloride and isooctyl fluroxypyr in sample by reversed phase high performance liquid chromatography, and can complete simultaneous detection of 2 methyl 4 isooctyl chloride and isooctyl fluroxypyr under the same chromatography condition by external standard method, with good separation effect and short peak time, while ensuring accuracy and improving detection efficiency.
Drawings
FIG. 1 is an HPLC chart of isooctyl 2-methyl-4-chlorohydrate and isooctyl fluroxypyr-meptyl in example 1;
FIG. 2 is a linear correlation curve of isooctyl fluroxypyr;
FIG. 3 is a linear correlation curve for isooctyl 2-methyl-4-chloride;
FIG. 4 is a HPLC chart obtained by taking 48% 2-methyl chloride bifluoride suspoemulsion as a sample in example 2;
FIG. 5 is a HPLC chart obtained by taking 48% 2-methyl chloride bifluoride suspoemulsion as a sample in example 3;
FIG. 6 is an HPLC chart obtained by taking 48% 2-methyl chloride bifluoride suspoemulsion as a sample in example 4.
Detailed Description
The present invention will be further described with reference to examples and drawings, but the present invention is not limited to the examples.
Example 1
1. Detection of
(1) Preparing a standard solution: accurately weighing 0.05g (0.0001 g accurate) of 2-methyl-4-chloroisooctyl ester standard sample and 0.05g (0.0001 g accurate) of fluroxypyr-meptyl ester standard sample, placing into the same 50mL volumetric flask, diluting with acetonitrile to scale, completely dissolving by ultrasonic wave, and cooling to room temperature for standby;
(2) Preparing a sample solution: accurately weighing 0.05g (0.0001 g accurate) of each sample containing 2-methyl-4-chloroisooctyl ester and fluroxypyr-meptyl ester, placing the samples into a 50mL volumetric flask, diluting the samples to the scale with acetonitrile, completely dissolving the samples by ultrasonic waves, cooling the samples to room temperature, and filtering the samples by a 0.45 mu m filter membrane for later use;
(3) And (3) measuring:
chromatographic column: c18 column, 250 mm. Times.4.6 mm,5 μm,
mobile phase: acetonitrile-pH 3.0 phosphoric acid solution with the volume ratio of 82:18,
flow rate: 1.0mL/min of the total weight of the mixture,
column temperature: 35 c,
detection wavelength: at a wavelength of 235nm,
sample injection volume: 5. Mu.L of the gel was used,
under the chromatographic condition, after the instrument baseline is stable, continuously injecting a plurality of needles of standard solution, and respectively carrying out sample injection and peak area measurement according to the sequence of the standard solution, the sample solution and the standard sample solution when the relative change of the peak areas of 2 methyl 4 chloroisooctyl ester or fluroxypyr isooctyl ester of two adjacent needles is less than 1.5 percent;
(4) And (3) calculating: the average value of the areas of 2 methyl 4 chloroisooctyl ester or fluroxypyr-meptyl acetate Xin Zhifeng in the two-needle sample solution and the two-needle standard solution before and after the sample is calculated, and the mass fraction X of the 2 methyl 4 chloroisooctyl ester or fluroxypyr-meptyl acetate in the sample is calculated according to the following formula 1 ：
X 1 =
Wherein:
A 1 -average of peak areas of 2 methyl 4 chloroisooctyl ester or fluroxypyr meptyl in the standard solution;
A 2 -average of peak areas of 2 methyl 4 chloroisooctyl ester or fluroxypyr meptyl in the sample solution;
m 1 -2 methyl 4 chloroisooctyl ester or fluroxypyr-meptyl ester) standard mass, g;
m 2 sample mass, g;
the mass fraction of the 2-methyl-4-chloroisooctyl ester or the chlorofluopicolide in the P-standard sample is percent.
As a result, as shown in FIG. 1, peak No. 1 is isooctyl fluroxypyr, and the retention time is about 10.0min; peak 2 is 2 methyl 4 isooctyl chloride with a retention time of about 16.5min.
2. Specificity (specificity)
About 0.025g of standard sample of fluroxypyr and 0.05g of standard sample of 2-methyl-4-chloroisooctyl are weighed, placed in a 100mL volumetric flask, dissolved with acetonitrile and diluted to a scale, shaken well, filtered, and used as a specificity-standard solution. About 0.17g of a sample containing fluroxypyr-meptyl ester and 2-methyl-4-chloroisooctyl ester was weighed, placed in a 100mL volumetric flask, diluted to scale with acetonitrile, shaken well, and filtered as a specificity-sample solution. Under the chromatographic conditions, after the instrument is stable, the specificity-standard sample solution and the specificity-sample solution are sequentially injected for specificity measurement.
The results showed that no impurity was detected in the specificity-standard solution, and that fluroxypyr i Xin Zhifeng had a purity index of 1.000000,2 methyl 4 chloroi Xin Zhifeng of 1.000000; no impurities were detected in the specificity-sample solution, and the purity index of fluroxypyr-meptyl-acetate Xin Zhifeng was 1.000000,2 and that of methyl 4-chloroiso Xin Zhifeng was 1.000000, indicating that the specificity was satisfactory.
3. Linear correlation
0.0506g of standard sample of fluroxypyr and 0.1018g of standard sample of 2-methyl-4-chloroisooctyl are weighed, placed in a 50mL volumetric flask, dissolved and diluted to a scale with acetonitrile, shaken uniformly and filtered to obtain standard mother liquor. 1.0mL, 2.0mL, 4.0mL, 6.0mL and 10.0mL of the standard sample mother solution are respectively removed by a pipette and are put into a 10mL volumetric flask, and are diluted to the scale by acetonitrile, and are uniformly shaken, wherein 5 standard sample solutions with linear concentration are used as linear related solutions. Under the chromatographic conditions, after the instrument is stabilized, linear correlation solutions with different concentrations are added for linear correlation measurement.
A linear regression curve was drawn with the concentration of isooctyl fluroxypyr as the abscissa and the peak area of isooctyl fluroxypyr as the ordinate (FIG. 2). The results show that the concentration of the fluroxypyr-meptyl has good linearity between 0.1002g/L and 1.002g/L, and the concentration of the fluroxypyr-meptyl corresponds to chlorineA good linear equation is presented between the peak areas of the isooctyl fluroxypyr. The linear equation is y= 53399381 x+ 512285, and the linear correlation coefficient r 2 =1.0000, greater than the limit of 0.99, indicating that the linear correlation confirmed by the fluroxypyr isooctyl ester analysis method is satisfactory. Similarly, a linear regression curve was drawn with the concentration of 2 methyl 4 chloroisooctyl ester on the abscissa and the peak area of 2 methyl 4 chloroisooctyl ester on the ordinate (FIG. 3). The results show that the concentration of 2-methyl-4-chloroisooctyl ester has good linearity between 0.2016g/L and 2.0156g/L, and a good linear equation is presented between the peak areas of the corresponding 2-methyl-4-chloroisooctyl esters. The linear equation is y= 16732920 x+ 369016, and the linear correlation coefficient r 2 =1.0000, greater than the limit value 0.99. Indicating that the linear correlation confirmed by the analysis method of the 2-methyl-4-chloroisooctyl ester meets the requirement.
4. Accuracy of
Taking 5 50mL volumetric flasks, adding a certain amount of isooctyl fluroxypyr and 2-methyl-4-chloroisooctyl standard sample into each volumetric flask, fixing the volume by using a sample solution, and filtering to obtain 5 solutions as accurate solutions. Preparing a mixed sample solution with medium concentration as a standard sample solution, and sampling according to the following sequence after the instrument is stable: and (5) performing accuracy measurement on the standard sample solution, the accuracy solution and the standard sample solution.
TABLE 1 determination of accuracy of fluroxypyr-meptyl ester
Table 22 determination of accuracy of methyl 4 chloroisooctyl ester
From the data in tables 1 and 2, the average recovery rate of the fluroxypyr ester is 99.40 percent, and the average recovery rate is between 98 percent and 101 percent, which shows that the accuracy confirmed by the fluroxypyr ester analysis method meets the requirement; the average recovery rate of the 2-methyl-4-chloroisooctyl ester is 99.62 percent and is between 98 percent and 101 percent, which shows that the accuracy confirmed by the analysis method of the 2-methyl-4-chloroisooctyl ester meets the requirement.
5. Precision of
0.17g (accurate to 0.0001 g) of a sample containing 2-methyl-4-chloroisooctyl acetate and 0.16g (accurate to 0.0001 g) of a sample containing chlorofluoro-pyriloxy acetate are respectively weighed accurately, 5 parts are placed in a 50-mL volumetric flask, diluted to a scale with acetonitrile and shaken uniformly, and the 5 sample solutions are used as precision solutions. And taking the mixed sample solution with medium concentration as a standard sample solution, and sampling according to the following sequence after the instrument is stable: and (5) performing precision measurement on the standard sample solution, the precision solution and the standard sample solution.
TABLE 3 determination of precision of fluroxypyr-meptyl ester
Table 4 2 determination results of precision of methyl 4-chloroisooctyl ester
From the data in tables 3 and 4, the relative standard deviation of the mass fraction measurement of the fluroxypyr-meptyl is 0.67 percent and is smaller than the limit value of 1.60 percent, which indicates that the precision confirmed by the fluroxypyr-meptyl analysis method meets the requirements; the relative standard deviation of the mass fraction measurement of the 2-methyl-4-chloroisooctyl ester is 0.74 percent and is smaller than the limit value of 1.76 percent, which shows that the precision confirmed by the analysis method of the 2-methyl-4-chloroisooctyl ester meets the requirement.
Example 2
Measurement of 48% 2-methyl chloride bifluoride suspoemulsion (35.6% +12% + 0.4%) was carried out as in example 1, wherein the preparation of the sample solution of step (2) was replaced by the following method:
accurately weighing 0.17g (accurate to 0.0001 g) of a 48% 2-methyl chloride bifluoride suspension emulsion sample, placing the suspension sample in a 50mL volumetric flask, diluting the suspension sample to a scale with acetonitrile, completely dissolving the suspension sample by ultrasonic waves, cooling the suspension sample to room temperature, and filtering the suspension sample by a 0.45 mu m filter membrane for later use.
The obtained chromatogram is shown in fig. 4: peak No. 2 is fluroxypyr ester with a retention time of about 10.0 minutes; peak 3 is 2 methyl 4 isooctyl chloride with a retention time of about 16.5min. The content of the fluroxypyr ester in the sample was calculated to be 12.2% w/w and the content of the 2-methyl-4-chloroisooctyl ester was calculated to be 35.8% w/w.
Example 3
A 48% 2 methyl chloride bifluoride suspoemulsion (35.6% +12% + 0.4%) assay was performed as in example 2, wherein the assay of step (3) was replaced by the following method:
chromatographic column: c18 column, 250 mm. Times.4.6 mm,5 μm,
mobile phase: acetonitrile-pH 3.5 phosphoric acid solution with the volume ratio of 80:20,
flow rate: 1.0mL/min of the total weight of the mixture,
column temperature: 30 ℃,
detection wavelength: at a wavelength of 235nm,
sample injection volume: 5. Mu.L.
The obtained chromatogram is shown in fig. 5: the retention time of the fluroxypyr-meptyl ester is about 12 minutes; the retention time of 2-methyl-4-chloroisooctyl ester was about 21min. The content of the fluroxypyr ester in the sample was calculated to be 12.2% w/w and the content of 2-methyl-4-chloroisooctyl ester was calculated to be 35.7% w/w.
Example 4
A 48% 2 methyl chloride bifluoride suspoemulsion (35.6% +12% + 0.4%) assay was performed as in example 2, wherein the assay of step (3) was replaced by the following method:
chromatographic column: c18 column, 250 mm. Times.4.6 mm,5 μm,
mobile phase: acetonitrile-pH 3.0 phosphoric acid solution with the volume ratio of 85:15,
flow rate: 1.0mL/min of the total weight of the mixture,
column temperature: 35 c,
detection wavelength: at a wavelength of 235nm,
sample injection volume: 5. Mu.L.
The obtained chromatogram is shown in fig. 6: the retention time of the fluroxypyr-meptyl ester is about 8 minutes; the retention time of 2-methyl-4-chloroisooctyl ester was about 14.5min. The content of the fluroxypyr ester in the sample was calculated to be 12.3% w/w and the content of 2-methyl-4-chloroisooctyl ester was calculated to be 35.6% w/w.
Claims (3)
1. An HLPC method for detecting isooctyl 2-methyl-4-chloride and isooctyl fluroxypyr, comprising the steps of:
(1) Preparing a standard solution of 2 methyl 4-chloroisooctyl-fluroxypyr-meptyl;
(2) Obtaining a sample solution to be tested;
(3) The peak areas of the 2-methyl-4-chloroisooctyl-fluroxypyr standard solution and the sample solution to be tested are respectively measured under the following high performance liquid chromatography conditions:
chromatographic column: a C18 column, which is provided with a plurality of holes,
mobile phase: acetonitrile-pH 3-3.5 phosphoric acid solution with the volume ratio of 80:20-85:15,
flow rate: 0.8-1.5mL/min,
column temperature: 25-35 ℃,
detection wavelength: at a wavelength of 235nm,
sample injection volume: 5-10 mu L;
(4) Calculating the mass fraction of 2 methyl 4 chloroisooctyl ester or fluroxypyr-meptyl in the sample solution to be detected;
the sample to be detected is 48% 2 methyl chloride bifluoride suspoemulsion;
in the step (2), the obtaining step of the sample solution to be measured is as follows: and extracting the sample to be tested by acetonitrile and diluting.
2. HLPC process according to claim 1, characterized in that in step (3) the column packing has a particle size of 3-5 μm, a column length of 150-250mm and an inner diameter of 2-4.6mm.
3. HLPC method according to claim 1, characterized in that in step (4) the mass fraction X1 of 2 methyl 4 chloroisooctyl ester or fluroxypyr meptyl in the sample solution to be tested is calculated according to the following formula:
X1=
wherein:
a1-peak area of 2 methyl 4 chloroisooctyl ester or fluroxypyr meptyl in the standard sample solution;
a2-peak area of 2 methyl 4 chloroisooctyl ester or fluroxypyr-meptyl in sample solution;
m 1-2 methyl 4 chloroisooctyl ester or fluroxypyr-meptyl standard sample mass g;
m2, the mass of the sample, g;
p-mass percent of 2 methyl 4 chloroisooctyl ester or chlorofluopicolide in the standard sample.
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| 2甲4氯·氯氟吡36%可湿性粉剂高效液相色谱分析;文师倩 等;农药科学与管理;第34卷(第5期);50-52 * |
| Determination of acidic herbicides in cereals by QuEChERS extraction and LC/MS/MS;ANGELA SANTILIO 等;Journal of Environmental Science and Health;第46卷;535-543 * |
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