CN108760943B - Method for detecting content of cyhalofop-butyl and pyribenzoxim in compound preparation - Google Patents
Method for detecting content of cyhalofop-butyl and pyribenzoxim in compound preparation Download PDFInfo
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- CN108760943B CN108760943B CN201810934389.5A CN201810934389A CN108760943B CN 108760943 B CN108760943 B CN 108760943B CN 201810934389 A CN201810934389 A CN 201810934389A CN 108760943 B CN108760943 B CN 108760943B
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- pyribenzoxim
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- butyl
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Abstract
The invention provides a method for detecting the content of cyhalofop-butyl and pyribenzoxim in a compound preparation, which comprises the following steps: detecting a sample to be detected of the compound preparation of cyhalofop-butyl and pyribenzoxim by high performance liquid chromatography to obtain the content of cyhalofop-butyl and the content of pyribenzoxim; the wavelength detected by the high performance liquid chromatography is selected to be 225-240 nm; the mobile phase detected by the high performance liquid chromatography is a mixture of acetonitrile and water, and the volume ratio of the acetonitrile to the water is (58-62) to (38-42), so that the detection can be performed without pretreating a compound preparation of cyhalofop-butyl and pyribenzoxim, and the detection result is accurate, good in reproducibility and high in sensitivity.
Description
Technical Field
The invention relates to the field of analytical chemistry, and particularly relates to a method for detecting the content of cyhalofop-butyl and pyribenzoxim in a compound preparation.
Background
The cyhalofop-butyl and pyribenzoxim compound emulsifiable concentrate or compound oil suspension is a compound herbicide and has obvious weeding effect on gramineous weeds. At present, no relevant patent is found in the method for measuring the content of cyhalofop-butyl and the content of pyribenzoxim at home and abroad, the method for detecting the cyhalofop-butyl component is a high performance liquid chromatography forward detection method, the method for detecting the pyribenzoxim component is a high performance liquid chromatography reverse detection method, the method disclosed at present is long in time consumption and wastes reagents when being used for independently detecting each component, and the impurity peak and the effective component peak can not be separated according to the detection method. Therefore, in order to develop the use of the cyhalofop-butyl and pyribenzoxim compound preparation, the method for detecting the content of the cyhalofop-butyl and the pyribenzoxim in the cyhalofop-butyl and pyribenzoxim compound preparation has important significance.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide a method for detecting the content of cyhalofop-butyl and pyribenzoxim in a compound preparation, the method provided by the invention does not need to process the compound reagent to be detected, and the method has the advantages of accurate detection result, high sensitivity and good reproducibility.
The invention provides a method for detecting the content of cyhalofop-butyl and pyribenzoxim in a compound preparation, which comprises the following steps:
detecting a sample to be detected of the compound preparation of cyhalofop-butyl and pyribenzoxim by high performance liquid chromatography to obtain the content of cyhalofop-butyl and the content of pyribenzoxim;
wherein the wavelength of the high performance liquid chromatography detection is 225-240 nm;
the mobile phase detected by the high performance liquid chromatography is a mixture of acetonitrile and water, and the volume ratio of the acetonitrile to the water is (58-62) to (38-42).
Preferably, the chromatographic column for high performance liquid chromatography detection is a bonded stationary phase chromatographic column.
Preferably, the bonded stationary phase chromatographic column is a C30, C18, C8 or C4 column.
Preferably, the length of the chromatographic column is 1-1000 mm.
Preferably, the inner diameter of the chromatographic column is 0.1-50 mm.
Preferably, the volume ratio of acetonitrile to water is preferably 58:42, 59:41, 60: 40, 61: 39 or 62: 38.
Preferably, the flow rate of the mobile phase is 0.8-1.2 mL/min.
Preferably, the flow rate of the mobile phase is 1 mL/min.
Preferably, the compound preparation to be tested of cyhalofop-butyl and pyribenzoxim is prepared according to the following method:
and mixing the compound preparation of cyhalofop-butyl and pyribenzoxim with acetonitrile to obtain a sample to be tested of the compound preparation of cyhalofop-butyl and pyribenzoxim.
Preferably, the compound preparation of cyhalofop-butyl and pyribenzoxim is a compound emulsifiable concentrate preparation of cyhalofop-butyl and pyribenzoxim or a compound oil suspension of cyhalofop-butyl and pyribenzoxim.
Compared with the prior art, the invention provides a method for detecting the content of cyhalofop-butyl and pyribenzoxim in a compound preparation, which comprises the following steps: detecting a sample to be detected of the compound preparation of cyhalofop-butyl and pyribenzoxim by high performance liquid chromatography to obtain the content of cyhalofop-butyl and the content of pyribenzoxim; the wavelength detected by the high performance liquid chromatography is selected to be 225-240 nm; the mobile phase detected by the high performance liquid chromatography is a mixture of acetonitrile and water, and the volume ratio of the acetonitrile to the water is (58-62) to (38-42), so that the detection can be performed without pretreating a compound preparation of cyhalofop-butyl and pyribenzoxim, and the detection result is accurate, good in reproducibility and high in sensitivity.
Drawings
FIG. 1 is a chromatogram of a standard solution of cyhalofop-butyl and pyribenzoxim;
FIG. 2 is a chromatogram of a sample to be tested of cyhalofop-butyl and pyribenzoxim emulsifiable concentrate;
FIG. 3 is a chromatogram obtained when the volume ratio of acetonitrile and water in a mobile phase is 55: 45 of a sample to be tested of cyhalofop-butyl and pyribenzoxim emulsifiable concentrate;
FIG. 4 is a chromatogram obtained when the volume ratio of acetonitrile and water in a mobile phase is 65: 35 of a sample to be tested of cyhalofop-butyl and pyribenzoxim emulsifiable concentrate;
FIG. 5 is a chromatogram obtained when the volume ratio of acetonitrile and water in the mobile phase is 70: 30 for a sample to be tested of cyhalofop-butyl and pyribenzoxim emulsifiable concentrate.
Detailed Description
The invention provides a method for detecting the content of cyhalofop-butyl and pyribenzoxim in a compound preparation, which comprises the following steps:
detecting a sample to be detected of the compound preparation of cyhalofop-butyl and pyribenzoxim by high performance liquid chromatography to obtain the content of cyhalofop-butyl and pyribenzoxim;
wherein the wavelength detected by the high performance liquid chromatography is 225-240 m;
the mobile phase detected by the high performance liquid chromatography is a mixture of acetonitrile and water, and the volume ratio of the acetonitrile to the water is (58-62) to (38-42).
In the invention, the chromatographic column for high performance liquid chromatography detection is preferably a bonded stationary phase chromatographic column, and more preferably a C30, C18, C8 or C4 column; wherein the inner diameter of the chromatographic column is preferably 0.1-50 mm, more preferably 1-10 mm, and more preferably 4.6-6 mm; the length of the chromatographic column is preferably 1-1000 mm, more preferably 200-800 mm, and most preferably 232-500 mm; the granularity of the chromatographic column packing is preferably 0.1-20 μm, and more preferably 5.0-10 μm.
In the invention, the detector for detecting the high performance liquid chromatography is preferably a variable wavelength ultraviolet detector; the wavelength of the high performance liquid chromatography detection is preferably 225-240 nm, and more preferably 232 nm.
In the present invention, the volume ratio of acetonitrile to water is preferably 58:42, 59:41, 60: 40, 61: 39 or 62:38, and more preferably 60: 40. The flow rate of the mobile phase is preferably 0.8-1.2 mL/min, and more preferably 1 mL/min.
In the invention, the compound preparation to be tested of cyhalofop-butyl and pyribenzoxim is prepared according to the following method: and mixing the compound preparation of cyhalofop-butyl and pyribenzoxim with acetonitrile to obtain a sample to be tested of the compound preparation of cyhalofop-butyl and pyribenzoxim. The invention has no special requirements on the formulation of the compound preparation, such as a cyhalofop-butyl and pyribenzoxim compound missible oil preparation or a cyhalofop-butyl and pyribenzoxim compound oil suspension.
In the present invention, the sample amount of the sample to be measured is preferably 5. mu.L. The calculation method of the sample to be measured is preferably obtained by calculation by adopting an external standard method.
The method for detecting the content of cyhalofop-butyl and pyribenzoxim in the compound preparation provided by the invention comprises the steps of detecting a sample to be detected of the compound preparation of cyhalofop-butyl and pyribenzoxim by high performance liquid chromatography to obtain the content of cyhalofop-butyl and pyribenzoxim in the compound preparation; the wavelength detected by the high performance liquid chromatography is selected to be 225-240 nm; the mobile phase detected by the high performance liquid chromatography is a mixture of acetonitrile and water, and the volume ratio of the acetonitrile to the water is (58-62) to (38-42), so that the detection can be performed without pretreatment and interference discharge of a compound preparation of cyhalofop-butyl and pyribenzoxim, the detection process of the high performance liquid chromatography is greatly simplified, and the detection result is accurate, the reproducibility is good, and the sensitivity is high.
The following will clearly and completely describe the technical solutions of the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The instruments used in each example are Shimadzu LC-20A high performance liquid chromatograph; the cyhalofop-butyl and pyribenzoxim standards are Fluka standards.
Example 1
The chromatographic conditions tested were as follows:
variable wavelength ultraviolet detector, C18 chromatography column 5.0 μm250mm × 4.6mm (i.d.);
mobile phase: acetonitrile and water 60: 40;
detection wavelength: 232 nm;
flow rate: 1.0 mL/min;
the specific detection method comprises the following steps:
accurately weighing 0.05g of cyhalofop-butyl serving as a standard substance and 0.0210g of pyribenzoxim serving as pyribenzoxim, putting the cyhalofop-butyl and the pyribenzoxim serving as a standard substance into the same 50mL volumetric flask, dissolving the cyhalofop-butyl and the pyribenzoxim with acetonitrile, and diluting the solution to the scale mark. Weighing about 0.8100g of a sample of the 60g/L cyhalofop-butyl and 25g/L pyribenzoxim compound missible oil, placing the sample in a 50mL volumetric flask, dissolving and diluting the sample to the scale with acetonitrile, and degassing for 5 minutes by ultrasonic waves. And (3) carrying out liquid chromatography analysis on a standard sample, wherein the sample amount is 5 mu L, and determining peak areas of cyhalofop-butyl and pyribenzoxim. A sample was subjected to liquid chromatography with a sample volume of 5. mu.L for detection. The chromatogram of the cyhalofop-butyl and pyribenzoxim standard solution is shown in figure 1, figure 1 is the chromatogram of the cyhalofop-butyl and pyribenzoxim standard solution, and it can be seen from the figure that 32.5min is the peak of cyhalofop-butyl and 44.1min is the peak of pyribenzoxim. The chromatogram of a sample to be tested of the cyhalofop-butyl and pyribenzoxim missible oil is shown in figure 2, and figure 2 is the chromatogram of the sample to be tested of the cyhalofop-butyl and pyribenzoxim missible oil, so that the peak emergence time of a main peak is appropriate, the separation degree of the main peak and a mixed peak is good, and the content of the cyhalofop-butyl and the pyribenzoxim in the sample is respectively calculated by an external standard method to be 5.67 percent and 2.36 percent.
And adding the standard products of cyhalofop-butyl and pyribenzoxim into the sample solution, performing four standard adding contents on the sample according to the experimental conditions, performing 3 times of parallel measurement on each standard adding content to obtain an average value, wherein the result is shown in table 1, and the standard adding recovery rate of the sample is calculated to be between 99% and 101% according to the actual adding amount and the actual measurement result.
TABLE 1
Example 2
In order to verify the feasibility and the accuracy of the detection method in example 1, a precision test was performed, which used a standard solution of cyhalofop-butyl and pyribenzoxim prepared at a concentration of 1000mg/L, and 5 μ L of the standard solution was continuously injected for 6 times, and the measurement results are shown in table 2.
TABLE 2
| Serial number | Peak area of cyhalofop-butyl | Peak area of pyribenzoxim |
| 1 | 35305737 | 19577492 |
| 2 | 35378562 | 19629415 |
| 3 | 35309456 | 19584366 |
| 4 | 35287942 | 19507963 |
| 5 | 35432953 | 19459937 |
| 6 | 35407689 | 19566193 |
| Mean value of | 35353723 | 19554228 |
| RSD％ | 0.16 | 0.28 |
From Table 2, it can be seen that the RSD of the peak area is less than 2%, and therefore the method is stable.
Example 3
To better illustrate the stability of the sample solutions containing cyhalofop-butyl and pyribenzoxim provided in the examples of the present invention, the sample solutions were prepared and then left for 4h, 8h, 12h and 24h respectively for liquid chromatography, and the results are shown in table 3.
TABLE 3
As can be seen from Table 3, the RSD of the peak area is less than 2%, and the stability of the test solution provided by the invention is good.
Comparative example 1
The method of example 1 is used for detecting 60g/L cyhalofop-butyl and 25g/L pyribenzoxim compound missible oil, the volume ratio of acetonitrile and water of a mobile phase is changed, other detection conditions and detection methods are not changed, and the results are as follows:
mobile phase: when the volume ratio of acetonitrile to water is 55: 45, the obtained chromatogram is shown in figure 3, figure 3 is the chromatogram obtained when the volume ratio of acetonitrile to water is 55: 45 of a sample to be detected of cyhalofop-butyl and pyribenzoxim missible oil is mobile phase acetonitrile to water, and as can be seen from the chromatogram, the peak with the retention time of 71.8min is cyhalofop-butyl, and the peak with the retention time of 110.08min is pyribenzoxim, the detection time consumption under the mobile phase condition can be increased by one time.
Mobile phase: when the volume ratio of acetonitrile to water is 65: 35, the obtained chromatogram is shown in figure 4, figure 4 is the chromatogram obtained when the volume ratio of acetonitrile to water is 65: 35 of a sample to be tested of cyhalofop-butyl and pyribenzoxim missible oil is mobile phase acetonitrile to water, and as can be seen from the chromatogram, the peak with the retention time of 22.5min is cyhalofop-butyl, the peak with the retention time of 26.5min is pyribenzoxim, the peak of pyribenzoxim is completely coincided with the impurity peak, and the target peak can not be separated under the mobile phase.
Mobile phase acetonitrile: when the volume ratio of water is 70: 30, the obtained chromatogram is shown in figure 5, figure 5 is the chromatogram obtained when the volume ratio of acetonitrile to water in a mobile phase of a sample to be tested of cyhalofop-butyl and pyribenzoxim missible oil is 70: 30, and as can be seen from the figure, the retention time of cyhalofop-butyl in the mobile phase is 15.2min, the retention time of pyribenzoxim is 19.3min, the target peak can be seen to be completely coincided with the impurity peak in the chromatogram, and the target peak can not be separated at all in the mobile phase.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (8)
1. A method for detecting the content of cyhalofop-butyl and pyribenzoxim in a compound preparation comprises the following steps:
detecting a sample to be detected of the compound preparation of cyhalofop-butyl and pyribenzoxim by high performance liquid chromatography to obtain the content of cyhalofop-butyl and the content of pyribenzoxim;
wherein the wavelength of the high performance liquid chromatography detection is 225-240 nm;
the mobile phase detected by the high performance liquid chromatography is a mixture of acetonitrile and water, and the volume ratio of the acetonitrile to the water is (58-62): (38-42); the chromatographic column for high performance liquid chromatography detection is a bonded stationary phase chromatographic column, the bonded stationary phase chromatographic column is C18, and the filler granularity is 5.0 mu m.
2. The method of claim 1, wherein the column length of the chromatography column is 200 to 800 mm.
3. The method according to claim 1, wherein the inner diameter of the chromatographic column is 1 to 10 mm.
4. The method of claim 1, wherein the volume ratio of acetonitrile to water is 58:42, 59:41, 60: 40. 61: 39 or 62: 38.
5. The method according to claim 1, wherein the flow rate of the mobile phase is 0.8 to 1.2 mL/min.
6. The method of claim 1, wherein the flow rate of the mobile phase is 1 mL/min.
7. The method according to claim 1, wherein the compounded preparation of cyhalofop-butyl and pyribenzoxim to be tested is prepared according to the following method:
and mixing the compound preparation of cyhalofop-butyl and pyribenzoxim with acetonitrile to obtain a sample to be tested of the compound preparation of cyhalofop-butyl and pyribenzoxim.
8. The method according to claim 1, wherein the compound preparation of cyhalofop-butyl and pyribenzoxim is a compound emulsifiable concentrate preparation of cyhalofop-butyl and pyribenzoxim or a compound oil suspension of cyhalofop-butyl and pyribenzoxim.
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| JP2009046478A (en) * | 2007-07-25 | 2009-03-05 | Sumitomo Chemical Co Ltd | Imidate compound and application thereof for controlling noxious organism |
| CN102273459A (en) * | 2011-06-21 | 2011-12-14 | 王从爱 | Weeding composition containing pyribenzoxim and cyhalofopbutyl |
| WO2014023531A1 (en) * | 2012-08-07 | 2014-02-13 | Syngenta Participations Ag | Trifluoromethylpyridine carboxamides as pesticides |
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| CN107136056A (en) * | 2017-07-14 | 2017-09-08 | 安徽金农康农药检测有限公司 | A kind of pyribenzoxim and cyhalofop-butyl compounded cream and preparation method thereof |
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