Rapid quantitative detection method for pesticide fluridone

Abstract

This invention provides a rapid quantitative detection method for the pesticide flufenoxam, employing high-performance liquid chromatography (HPLC) for detection. The method includes the following steps: Step S1: Sample preparation; Step S2: Standard preparation; S3: Linearity test; Step S4: Sample detection; Qualitative analysis by retention time and quantitative analysis by external standard method. The chromatographic conditions are as follows: mobile phase: CH3CN:H2O = 60:40 (volume ratio); column: C18 column; column temperature: 30℃; flow rate: 1.0 mL / min; detection wavelength: 254 nm. This invention develops a rapid quantitative detection method for the pesticide flufenoxam, applicable to the quantitative detection of flufenoxam and other formulations. The method is simple, provides good separation, is accurate, and has good reproducibility. Flufenoxam concentration and peak area show a good linear relationship in the concentration range of 103.24 mg / L to 206.19 mg / L, and exhibit strong specificity.

Description

Technical Field

[0001] This invention relates to the field of fluroxypyr detection technology, specifically to a rapid quantitative detection method for the pesticide fluroxypyr. Background Technology

[0002] Fluxofeni, also known as oxadiazine, has the molecular formula C60. 12 H 11 ClF3NO3, molecular weight 309.6690, molecular structure is:

[0003]

[0004] Fluroxypyr is registered for use on a variety of crops worldwide and is an excellent herbicide antidote. As a highly effective oxime ether herbicide safener, fluroxypyr is used on seeds and plants. Especially for seed treatment, fluroxypyr is an excellent herbicide antidote, protecting grains or forage sorghum from herbicides such as metolachlor. It also helps provide better weed control and care for crops and the environment.

[0005] Currently, the common formulations of fluroxypyr on the market are powder, emulsifiable concentrate, granules, and technical grade, but no methods for detecting the content of fluroxypyr have been reported. Summary of the Invention

[0006] The purpose of this invention is to overcome the shortcomings of the prior art and provide a rapid quantitative detection method for the pesticide fluroxypyr.

[0007] To achieve the above and other objectives, the present invention is implemented through the following technical solution: a rapid quantitative detection method for the pesticide fluroxypyr is provided, comprising the following steps:

[0008] Step S1: Sample preparation;

[0009] Weigh the sample to be tested into a volumetric flask and dissolve it in a solvent.

[0010] Step S2: Standard product configuration;

[0011] Weigh different masses of flufenoxam reference material into volumetric flasks, dissolve and dilute the reference material with solvent to prepare flufenoxam standards of different concentrations.

[0012] Step S3: Linearity test;

[0013] The fluroxypyr standard of different concentrations prepared in step S2 was determined by high performance liquid chromatography under certain conditions, and the detection data were fitted to obtain linear curves and linear equations.

[0014] Step S4: Sample testing;

[0015] The sample to be tested prepared in step S1 is subjected to high performance liquid chromatography for detection and determination, with retention time for qualitative analysis and external standard method for quantitative analysis.

[0016] The conditions for detection by high performance liquid chromatography are as follows:

[0017]

[0018] In one embodiment, the retention times of fluazinam were 5.3 min and 5.5 min, respectively.

[0019] In one embodiment, the solvent is acetonitrile, and the acetonitrile is of chromatographic purity.

[0020] In one embodiment, step S2 includes:

[0021] Step S21: Prepare standard stock solution;

[0022] Weigh 50±3 mg of flufenoxam standard into a clean 100.0 mL volumetric flask, add acetonitrile to dissolve it completely, make up to volume and shake well to prepare the standard stock solution, denoted as S solution.

[0023] Step S22, preparation of linear solution;

[0024] Accurately weigh 35±3 mg, 45±3 mg, 55±3 mg and 65±3 mg of flufenoxam standard into clean 100.0 mL volumetric flasks, dilute to volume with acetonitrile and shake well to prepare linear solutions, wherein the linear solutions also include the S solution.

[0025] In one embodiment, the linear curve plotting in step S3 includes:

[0026] Step S31: Pipette 1.5 mL of blank solution and 1.5 mL of linear solutions of different concentrations prepared in step S22 into injection vials, and perform detection using high performance liquid chromatography.

[0027] Step S32: Read the data obtained in step S31, plot a standard curve with concentration as the abscissa and peak area as the ordinate, and record the obtained linear equation and linear correlation coefficient.

[0028] In one embodiment, the blank solution is acetonitrile.

[0029] In one embodiment, the chromatographic column has dimensions of 250 mm × 4.6 mm × 5 μm.

[0030] The present invention has the following beneficial effects:

[0031] This invention develops a rapid quantitative detection method for the pesticide flufenoxam. This method is simple, has good separation effect, is accurate and reproducible, and can be used for the quantitative detection of flufenoxam and other formulations. The concentration of flufenoxam and the peak area show a good linear relationship in the concentration range of 103.24 mg / L to 206.19 mg / L, and it has strong specificity. Attached Figure Description

[0032] Figure 1 The image shows the detection chromatogram of T-1 in the quantitative detection experiment of this invention.

[0033] Figure 2 The image shows the chromatogram of T-2 in the quantitative detection experiment of this invention.

[0034] Figure 3 The image shows the chromatogram of S-1 detected in the quantitative detection experiment of this invention.

[0035] Figure 4 The image shows the chromatogram of S-2 detection in the quantitative detection experiment of this invention.

[0036] Figure 5 The image shows the chromatogram of L-1 detection in the linear verification experiment of this invention.

[0037] Figure 6 The image shows the chromatogram of L-2 detection in the linear verification experiment of this invention.

[0038] Figure 7 The image shows the chromatogram of L-3 detection in the linearity verification experiment of this invention.

[0039] Figure 8 The image shows the detection chromatogram of L-4 in the linear verification experiment of this invention.

[0040] Figure 9 The image shows the detection chromatogram of L-5 in the linearity verification experiment of this invention.

[0041] Figure 10 The image shown is a graph of the linear curve fitting in the linear verification experiment of this invention. Detailed Implementation

[0042] Please see Figures 1 to 10 The following specific examples illustrate the implementation of the present invention. Those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. It should be understood that many specific details are set forth in the following description to provide a thorough understanding of the present invention; however, the present invention may also be implemented in other ways different from those described herein. Therefore, the scope of protection of the present invention is not limited to the specific embodiments disclosed below.

[0043] This invention provides a rapid quantitative detection method for the pesticide fluroxypyr, which uses high-performance liquid chromatography (HPLC) for detection and external standard method for quantitative analysis, including the following steps:

[0044] Step S1: Sample preparation;

[0045] Weigh the sample to be tested into a volumetric flask and dissolve it using acetonitrile as the solvent.

[0046] Step S2: Standard product configuration;

[0047] Different masses of flufenoxam reference material were weighed into volumetric flasks, and acetonitrile was used as the solvent to dissolve and dilute the reference material to prepare flufenoxam standards of different concentrations.

[0048] Step S3: Linearity test;

[0049] The fluroxypyr standard of different concentrations prepared in step S2 was determined by high performance liquid chromatography under certain conditions, and the detection data were fitted to obtain linear curves and linear equations.

[0050] Step S4: Sample testing;

[0051] The sample to be tested prepared in step S1 is subjected to high performance liquid chromatography for detection and determination, with retention time for qualitative analysis and external standard method for quantitative analysis.

[0052] Furthermore, the conditions for high-performance liquid chromatography (HPLC) detection are as follows:

[0053]

[0054] Because flufenoxam exists as an isomer, it appears as two chromatographic peaks in the detection chromatogram, with retention times of 5.3 min and 5.5 min, respectively.

[0055] Preferably, all acetonitrile is of chromatographic grade.

[0056] Preferably, step S2 includes:

[0057] Step S21: Prepare standard stock solution;

[0058] Weigh 50±3 mg of flufenoxam standard into a clean 100.0 mL volumetric flask, add acetonitrile to dissolve it completely, make up to volume and shake well to prepare the standard stock solution, denoted as S solution.

[0059] Step S22, preparation of linear solution;

[0060] Accurately weigh 35±3 mg, 45±3 mg, 55±3 mg and 65±3 mg of flufenoxam standard into clean 100.0 mL volumetric flasks, dilute to volume with acetonitrile and shake well to prepare linear solutions, which are respectively labeled L-1, L-2, L-4 and L-5; and use solution S directly as linear solution L-3.

[0061] Preferably, the standard curve plotting in step S3 includes:

[0062] Step S31: Pipette 1.5 mL of blank solution B and 1.5 mL of linear solutions (L-1 to L-5) of different concentrations prepared in step S22 into vials, and perform detection using high performance liquid chromatography.

[0063] Step S32: Read the data obtained in step S31, plot a standard curve with concentration as the abscissa and peak area as the ordinate, and record the obtained parameters such as linear equation, linear correlation coefficient, slope and intercept.

[0064] Preferably, in step S31, the blank solution is acetonitrile.

[0065] Preferably, the injection sequence and number of times for each solution in step S31 are performed according to Table 1.

[0066] Table 1. Linear Analysis Injection Procedure

[0067] sequence Solution name Number of injections sequence Solution name Number of injections 1 B 3 4 L-3 1 2 L-1 1 5 L-4 1 3 L-2 1 6 L-5 1

[0068] The present invention will be further described below with reference to specific embodiments.

[0069] Example 1:

[0070] This embodiment demonstrates rapid quantitative detection of the pesticide fluroxypyr using the following method:

[0071] Step S1, Sample preparation;

[0072] Accurately weigh two 0.05g portions of the sample to be tested and place them in two clean 100mL volumetric flasks. Dilute to volume with acetonitrile and shake well. Record these portions as T-1 and T-2, respectively.

[0073] Step S2, preparation of standard solution;

[0074] Accurately weigh two 0.05g portions of flufenoxuron standard into two clean 100mL volumetric flasks, dilute to volume with acetonitrile, and shake well. These flasks are labeled S-1 and S-2, respectively.

[0075] Step S3: Sample and standard solution detection;

[0076] T-1, T-2, S-1, and S-2 were detected according to the following chromatographic conditions and the injection sequence in Table 2.

[0077] Chromatographic conditions:

[0078]

[0079] Table 2 Sample Injection Procedure for Content Detection

[0080] sequence Solution name Number of injections sequence Solution name Number of injections 1 S-1 1 3 T-2 1 2 T-1 1 4 S-2 1

[0081] Step S4, calculation of fluroxypyr content;

[0082] The content of fluroxypyr in the sample was calculated using the following formula:

[0083]

[0084] in:

[0085] w: Mass fraction of flufenoxam in the sample, % w1: Mass fraction of flufenoxam in the standard solution, %

[0086] m1: Mass of sample, g; m2: Mass of standard, g

[0087] A1: Average peak area of ​​fluroxypyr in standard solution

[0088] A2: Average peak area of ​​fluroxypyr in the sample

[0089] In this embodiment, the chromatograms of T-1, T-2, S-1, and S-2 are as follows: Figures 1 to 4 As shown.

[0090] Example 2:

[0091] This embodiment verifies the linearity of the rapid quantitative detection method for the pesticide fluroxypyr provided by the present invention.

[0092] Weigh a certain amount of flufenoxam standard into a clean 100mL volumetric flask, mix well with acetonitrile, and prepare sequential solutions with concentrations of 103.24mg / L, 128.68mg / L, 148.14mg / L, 166.14mg / L, and 206.19mg / L, respectively, and label them L-1, L-2, L-3, L-4, and L-5; use acetonitrile as blank sample B, and detect blank sample B and sequential solutions (L-1 to L-5) under the chromatographic conditions in Example 1, according to the injection procedure in Table 3:

[0093] Table 3. Linear Analysis Injection Procedure

[0094] sequence Solution name Number of injections sequence Solution name Number of injections 1 B 3 4 L-3 1 2 L-1 1 5 L-4 1 3 L-2 1 6 L-5 1

[0095] The chromatograms of solutions L-1 to L-5 are as follows: Figures 5-9 As shown in Table 4, the peak areas of flufenoxam in chromatograms L-1 to L-5 were read respectively. A linear curve was plotted with concentration on the x-axis and peak area on the y-axis. The linear curve is shown in Table 4. Figure 10 As shown, the linear equation and correlation coefficient were obtained through fitting.

[0096] Table 4 Linear Analysis Data

[0097]

[0098]

[0099] From Table 4 and Figure 10 The regression equation for fluroxypyr concentration and peak area is: y = 25.602x - 87.193, with a correlation coefficient R0. 2 =0.9991, indicating that the concentration of flumetsulam and the peak area have a good linear relationship in the concentration range of 103.24 mg / L to 206.19 mg / L.

[0100] Example 3:

[0101] This embodiment verifies the precision of the rapid quantitative detection method for the pesticide fluroxypyr provided by the present invention.

[0102] Following the detection method in Example 1, the sequence solution L-3 from Example 2 was injected six times consecutively, and these were labeled SP-S-1, SP-S-2, SP-S-3, SP-S-4, SP-S-5, and SP-S-6, respectively. The results of the six detections are shown in Table 5.

[0103] Table 5 Precision verification results

[0104]

[0105] As shown in Table 5, the relative standard deviation (RSD) of the detection method provided by this invention is 0.0465%, which meets the precision requirements.

[0106] In summary, this invention provides a rapid quantitative detection method for the pesticide flufenoxam. This method is simple, has good separation effect, is accurate, and has good reproducibility. It can be used for the quantitative detection of flufenoxam and other formulations. The concentration of flufenoxam and the peak area show a good linear relationship in the concentration range of 103.24 mg / L to 206.19 mg / L, and it has strong specificity.

[0107] Although the invention has been described and illustrated in detail with reference to preferred embodiments, the invention is not limited to the disclosed examples, and those skilled in the art can derive other variations therefrom without departing from the scope of protection of the invention.

Claims

1. A method for rapid quantitative detection of the pesticide fluridone, characterized in that, Includes the following steps: Step S1: Sample preparation; Weigh the sample to be tested into a volumetric flask and dissolve the sample in a solvent. Step S2: Standard product configuration; Weigh different masses of flufenoxam reference material into volumetric flasks, dissolve and dilute the reference material with solvent to prepare flufenoxam standards of different concentrations; Step S3: Linearity test; The fluazinam standards of different concentrations prepared in step S2 were subjected to high performance liquid chromatography under specific conditions, and the detection data were fitted to obtain linear curves and linear equations. Step S4: Sample testing; The sample to be tested prepared in step S1 is subjected to high performance liquid chromatography for detection and determination, with retention time for qualitative analysis and external standard method for quantitative analysis. The conditions for detection by high performance liquid chromatography are as follows: The retention times of flurbimethoxam were 5.3 min and 5.5 min, respectively.

2. The method for rapid quantitative detection of the pesticide fluridone according to claim 1, characterized in that, The solvent is acetonitrile, and the acetonitrile is of chromatographic purity.

3. The method for rapid quantitative detection of the pesticide fluridone according to claim 1, characterized in that, Step S2 includes: Step S21: Prepare standard stock solution; Weigh 50±3 mg of flufenoxam standard into a clean 100.0 mL volumetric flask, add acetonitrile to dissolve it completely, dilute to volume and shake well to prepare the standard stock solution, denoted as S solution; Step S22, preparation of linear solution; Accurately weigh 35±3 mg, 45±3 mg, 55±3 mg and 65±3 mg of flufenoxam standard into clean 100.0 mL volumetric flasks, dilute to volume with acetonitrile and shake well to prepare linear solutions, wherein the linear solutions also include the S solution.

4. The rapid quantitative detection method for the pesticide fluroxypyr according to claim 3, characterized in that, The linear curve plotting in step S3 includes: Step S31: Pipette 1.5 mL of blank solution and 1.5 mL of linear solutions of different concentrations prepared in step S22 into injection vials, and perform detection using high performance liquid chromatography. Step S32: Read the data obtained in step S31, plot a standard curve with concentration as the abscissa and peak area as the ordinate, and record the obtained linear equation and linear correlation coefficient.

5. The rapid quantitative detection method for the pesticide fluroxypyr according to claim 4, characterized in that, The blank solution is acetonitrile.

6. The rapid quantitative detection method for the pesticide fluroxypyr according to claim 1, characterized in that, The chromatographic column has dimensions of 250 mm × 4.6 mm × 5 μm.

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