CN115201387A - A kind of analytical method of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester content - Google Patents

Abstract

The invention relates to the technical field of chemical analysis, in particular to an analysis method for the content of (E) -2- (2-bromomethylphenyl) -2-methoxyimino methyl acetate. The detection is carried out by adopting a high performance liquid chromatography, and comprises the following steps: preparing a standard substance solution and a sample solution to be detected; sequentially injecting samples into a high performance liquid chromatograph for analysis according to the sequence of a standard substance, a sample to be detected, the standard substance and the sample to be detected; calculating the average peak area of (E) -2- (2-bromomethylphenyl) -2-methoxyimino acetic acid methyl ester in the standard sample and the sample to be detected, and calculating the content of (E) -2- (2-bromomethylphenyl) -2-methoxyimino acetic acid methyl ester in the sample to be detected according to an external standard method formula. The analysis method has strong specificity, good repeatability and good precision, and is particularly suitable for quality control of intermediate products in the production process of pesticides, thereby meeting the production requirement of high-quality pesticide trifloxystrobin.

Description

A kind of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester content Analytical method

technical field

The invention relates to the technical field of chemical analysis, in particular to a method for analyzing the content of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester.

Background technique

Trioxystrobin broad-spectrum fungicides are a new class of fluorine-containing fungicides successfully developed from natural product Strobilurins as the leading compounds of fungicides. It has the characteristics of high efficiency, broad spectrum, protection, treatment, eradication, penetration, systemic activity, resistance to rain erosion, and long lasting effect. It has no cross-resistance with the existing fungicides, and has good activity against almost all fungal diseases. Trioxystrobin is suitable for wheat, barley, rye, triticale, grapes, apples, peanuts, bananas, vegetables, etc. Trioxystrobin has high toxicity and high risk to fish and aquatic organisms; low toxicity to birds, bees, silkworms, and earthworms; safe to crops, because it can be rapidly degraded in soil and water, so it is safe to the environment, so it is safe to use in soil and water. There are very large application prospects in the market.

The English name of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetate methyl ester is (E)-Methyl-2-(2-broMoMethylphenyl)-2-MethoxyiMinoacetate, and the molecular formula is C ₁₁ H ₁₂ BrNO ₃ has a molecular weight of 286.12 and a melting point of 45-48° C. It is easily soluble in organic solvents such as acetonitrile and methanol. (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester is a key intermediate of tristrobin, which produces (E)-2-(2 - Dibromomethylphenyl)-2-methoxyiminoacetic acid methyl ester impurity and (Z)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester isomer Impurities will seriously affect the quality and efficacy of trioxystrobin.

After consulting relevant documents at home and abroad, there is no report about (E)-2-(2-bromomethylphenyl)-2-methoxyiminomethyl acetate content detection method in the prior art, so in order to meet the requirements of high For the production requirements of the quality pesticide technical triclostrobin, it is necessary to provide a corresponding content analysis and detection method.

SUMMARY OF THE INVENTION

Aiming at the blank of the content detection technology of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester, the present invention provides a (E)-2-(2-bromo An analytical method for the content of methyl phenyl)-2-methoxyiminoacetic acid methyl ester, the analytical method has strong specificity, good precision, high recovery rate and good repeatability, and is especially suitable for the quality of pesticide technical intermediate products control.

The technical scheme of the present invention is as follows:

A method for analyzing the content of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester, which adopts high performance liquid chromatography to analyze, comprising the following steps:

(1) Dissolve the standard and the sample to be tested with methanol as a solvent to prepare the standard solution and the solution of the sample to be tested;

(2) The detection wavelength is set within the range of 230-270nm, and after the instrument baseline is stable, the samples are injected and analyzed in the order of standard product, sample to be tested, standard product, and sample to be tested. The chromatographic conditions include: the chromatographic column is C18 A reversed-phase chromatographic column, the column temperature is 30-50°C, the mobile phase is a mixed system of acetonitrile and 0.8% (v/v) glacial acetic acid aqueous solution, and the volume ratio of acetonitrile and glacial acetic acid aqueous solution is 40-60:60-40;

(3) Calculate the peak area average value of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the standard solution and the sample solution to be tested, and treat according to the external standard method formula Calculate the mass fraction of methyl (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetate in the test sample:

where:

A ₁ ——In the standard solution, (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester peak area average value;

A ₂ — in the sample solution to be tested, the peak area average value of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester;

m ₁ ——the quality of the standard product;

m ₂ - the mass of the sample to be tested;

P ₁ — the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the standard product;

X ₁ ——the mass fraction of methyl (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetate in the sample to be tested.

Further, the column length of the chromatographic column is 150 mm, the inner diameter of the column is 4.6 mm, and the particle size of the column is 5 μm.

Further, the temperature of the chromatographic column was 40°C.

Further, the detection wavelength of high performance liquid chromatography was set to 254 nm.

Further, the volume ratio of acetonitrile and glacial acetic acid aqueous solution is 50:50.

Further, the high-performance liquid chromatography conditions further include: the sample volume for each injection is 5 μL.

Further, the high performance liquid chromatography conditions further include: the flow rate of the mobile phase is 0.8-1.2 mL/min, preferably 1.0 mL/min.

The beneficial effect of the present invention is that,

The invention provides a brand-new method for detecting the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester, which solves the lack of special (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester high performance liquid chromatography detection method, using the above method to detect (E)-2-(2-bromomethyl) The mass fraction of methyl phenyl)-2-methoxyiminoacetate can realize the complete separation of the main peak from isomers and impurities, the chromatographic peak shape is good, the integral calculation results are accurate, the operability is good, and the obtained results are more accurate In time, it is especially suitable for the quality control of pesticide technical intermediate products, and has an important role and practical significance to ensure the quality of the final product tristrobin.

Description of drawings

Fig. 1 is the chromatogram of the standard solution in Example 1.

FIG. 2 is a chromatogram of the sample solution to be tested in Example 1. FIG.

3 is a chromatogram of the standard solution in Example 2.

4 is a chromatogram of the sample solution to be tested in Example 2.

FIG. 5 is a chromatogram of the standard solution in Example 3. FIG.

FIG. 6 is a chromatogram of the sample solution to be tested in Example 3. FIG.

FIG. 7 is a chromatogram of the standard solution in Comparative Example 1. FIG.

FIG. 8 is a chromatogram of the sample solution to be tested in Comparative Example 1. FIG.

FIG. 9 is a chromatogram of the standard solution in Comparative Example 2. FIG.

10 is a chromatogram of the sample solution to be tested in Comparative Example 2.

FIG. 11 is a linear relationship diagram in Test Example 4. FIG.

Detailed ways

In order to make those skilled in the art better understand the technical solutions of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described The embodiments are only some of the embodiments of the present invention, but not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

Example 1

The content of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester solution obtained by 301 batches of product 817kg in workshop is analyzed, including the steps:

(1) Accurately weigh 0.0598g of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester standard product, put it in a 100mL volumetric flask, add 80mL methanol, shake to dissolve Then, it was diluted to the mark with methanol to obtain _a standard solution for later use. %;

Accurately weigh 0.2687 g of the sample to be tested, put it in a 100 mL volumetric flask, add 80 mL of methanol, shake to dissolve, and dilute to the mark with methanol to obtain a solution of the sample to be tested for later use;

(2) A high performance liquid chromatograph is used, the chromatographic column is a C18 reversed-phase chromatographic column, the column length of the chromatographic column is 150 mm, the inner diameter of the column is 4.6 mm, and the column particle size is 5 μm; the temperature of the chromatographic column is 40 ° C; the mobile phase is acetonitrile A mixed system with 0.8% (v/v) glacial acetic acid aqueous solution, the volume ratio of acetonitrile and glacial acetic acid aqueous solution is 50:50; the sample volume for each injection is 5 μL, and the flow rate of the mobile phase is 1 mL/min; the detection wavelength is set to Set at 254nm.

(3) After the baseline of the instrument is stable, inject samples in the order of standard, sample to be tested, standard product, and sample to be tested, and calculate the (E)-2-(2-bromomethyl value of standard solution and sample solution to be tested, respectively. Phenyl)-2-methoxyiminoacetic acid methyl ester peak area average value, detection data as shown in table 1 below:

Table 1 embodiment 1 detection results

(4) Calculate the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the sample to be tested according to the formula of the external standard method, and the specific formula is as follows:

In the formula: A ₁ - in the standard solution, (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester peak area average value;

A ₂ — in the sample solution to be tested, the peak area average value of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester;

m ₁ ——the quality of the standard product;

m ₂ - the mass of the sample to be tested;

P ₁ — the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the standard product;

X ₁ ——the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the sample to be tested;

The mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the sample to be tested was calculated to be 21.33%.

FIG. 1 and FIG. 2 are the chromatograms of the standard substance and the sample to be tested in this embodiment, respectively. In Figure 1, the peak corresponding to the 11.270min position represents (E)-2-(2-dibromomethylphenyl)-2-methoxyiminoacetic acid methyl ester impurity, and the peak corresponding to the 6.956min position is (E) -2-(2-Bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester; in Figure 2, the peak corresponding to the 11.327min position represents (E)-2-(2-dibromomethylphenyl) )-2-methoxyiminoacetic acid methyl ester impurity, the corresponding peak at 11.994min represents Z isomer, and the corresponding peak at 6.994min is (E)-2-(2-bromomethylphenyl)-2 -Methoxyiminoacetate methyl ester.

Example 2

The content of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester of 108.3 g of the product obtained in the pilot test 20220215 was analyzed, including the following steps:

(1) Accurately weigh 0.0569g of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester standard product, put it in a 100mL volumetric flask, add 80mL methanol, shake to dissolve Then, it was diluted to the mark with methanol to obtain _a standard solution for later use. %;

Accurately weigh 0.0795 g of the sample to be tested, put it in a 100 mL volumetric flask, add 80 mL of methanol, shake to dissolve, and dilute to the mark with methanol to obtain a solution of the sample to be tested for later use;

(2) A high performance liquid chromatograph is used, the chromatographic column is a C18 reversed-phase chromatographic column, the column length of the chromatographic column is 150 mm, the inner diameter of the column is 4.6 mm, and the column particle size is 5 μm; the temperature of the chromatographic column is 40 ° C; the mobile phase is acetonitrile A mixed system with 0.8% (v/v) glacial acetic acid aqueous solution, the volume ratio of acetonitrile and glacial acetic acid aqueous solution is 50:50; the sample volume for each injection is 5 μL, and the flow rate of the mobile phase is 1 mL/min; the detection wavelength is set to Set at 254nm.

(3) After the baseline of the instrument is stabilized, inject the samples in the order of standard product, sample to be tested, standard product, and sample to be tested, and calculate the (E)-2-(2-bromomethyl of the standard solution and the sample solution to be tested, respectively. phenyl)-2-methoxyiminoacetic acid methyl ester peak area average, detection data as shown in Table 2 below:

Table 2 embodiment 2 detection results

(4) Calculate the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the sample to be tested according to the formula of the external standard method, and the specific formula is the same as in Example 1 , the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the sample to be tested is calculated to be 46.85%.

FIG. 3 and FIG. 4 are the chromatograms of the standard substance and the sample to be tested in this embodiment, respectively. In Figure 3, the peak corresponding to the 6.947min position is the characteristic peak of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester; in Figure 4, the peak corresponding to the 11.258min position It is (E)-2-(2-dibromomethylphenyl)-2-methoxyiminoacetic acid methyl ester impurity, the corresponding peak at 11.874min represents Z isomer, and the corresponding peak at 6.950min is ( E)-Methyl 2-(2-bromomethylphenyl)-2-methoxyiminoacetate.

Example 3

The content of methyl (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester obtained in batches of 264g in the pilot test 20220225 was analyzed, including the following steps:

(1) Accurately weigh 0.0395g of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester standard product, put it in a 100mL volumetric flask, add 80mL methanol, shake to dissolve Then, it was diluted to the mark with methanol to obtain _a standard solution for later use. %;

Accurately weigh 0.1038 g of the sample to be tested, put it in a 100 mL volumetric flask, add 80 mL of methanol, shake to dissolve, and dilute to the mark with methanol to obtain the sample solution to be tested for later use;

(2) A high performance liquid chromatograph is used, the chromatographic column is a C18 reversed-phase chromatographic column, the column length of the chromatographic column is 150 mm, the inner diameter of the column is 4.6 mm, and the column particle size is 5 μm; the temperature of the chromatographic column is 40 ° C; the mobile phase is acetonitrile A mixed system with 0.8% (v/v) glacial acetic acid aqueous solution, the volume ratio of acetonitrile and glacial acetic acid aqueous solution is 50:50; the sample volume for each injection is 5 μL, and the flow rate of the mobile phase is 1 mL/min; the detection wavelength is set to Set at 254nm.

(3) After the baseline of the instrument is stable, inject samples in the order of standard, sample to be tested, standard product, and sample to be tested, and calculate the (E)-2-(2-bromomethyl value of standard solution and sample solution to be tested, respectively. Phenyl)-2-methoxyiminoacetic acid methyl ester peak area average value, detection data as shown in Table 3 below:

Table 3 embodiment 3 detection results

(4) Calculate the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the sample to be tested according to the formula of the external standard method, and the specific formula is the same as in Example 1 , the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the sample to be tested is calculated to be 45.54%.

FIG. 5 and FIG. 6 are the chromatograms of the standard substance and the sample to be tested in this embodiment, respectively. In Figure 5, the peak corresponding to the 11.383min position represents (E)-2-(2-dibromomethylphenyl)-2-methoxyiminoacetic acid methyl ester impurity, and the peak corresponding to the 7.049min position represents (E) -2-(2-Bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester; in Figure 6, the peak corresponding to the 11.366min position represents (E)-2-(2-dibromomethylphenyl) )-2-methoxyiminoacetic acid methyl ester impurity, the peak corresponding to the 12.056min position represents the Z isomer, and the peak corresponding to the 7.018min position represents (E)-2-(2-bromomethylphenyl)-2 -Methoxyiminoacetate methyl ester.

Comparative Example 1

The standard solution and the sample solution to be tested in Example 1 were taken as detection objects.

(1) A high performance liquid chromatograph is used, the chromatographic column is a C18 reversed-phase chromatographic column, the column length of the chromatographic column is 150 mm, the inner diameter of the column is 4.6 mm, and the column particle size is 5 μm; the temperature of the chromatographic column is 40 ° C; the mobile phase is acetonitrile A mixed system with 0.8% (v/v) glacial acetic acid aqueous solution, the volume ratio of acetonitrile and glacial acetic acid aqueous solution is 65:35; the sample volume for each injection is 5 μL, and the flow rate of the mobile phase is 1 mL/min; the detection wavelength is set to Set at 254nm.

(2) After the baseline of the instrument is stable, inject the samples in the order of the standard, the sample to be tested, the standard product, and the sample to be tested, and calculate the (E)-2-(2-bromomethyl) of the standard solution and the sample solution to be tested, respectively. Phenyl)-2-methoxyiminoacetic acid methyl ester peak area average value, detection data as shown in the following table 4:

Table 4 test results of comparative example 1

(3) calculate the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the sample to be tested according to the formula of external standard method, and the specific formula is the same as that in Example 1 , the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the sample to be tested is calculated to be 21.50%.

FIG. 7 and FIG. 8 are the chromatograms of the standard substance and the sample to be tested in this embodiment, respectively. In Figure 7, the peak corresponding to the 5.151min position is (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester, and the peak corresponding to the 9.584min position is (E)-2 -(2-dibromomethylphenyl)-2-methoxyiminoacetic acid methyl ester impurity; the corresponding peak at 5.139min in Figure 8 is (E)-2-(2-bromomethylphenyl)- 2-Methoxyiminoacetic acid methyl ester, the peak corresponding to the 9.595min position is (E)-2-(2-dibromomethylphenyl)-2-methoxyiminoacetic acid methyl ester impurity, 10.424min position The corresponding peak is the Z isomer. Through this comparative example, it is found that the main peak of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester is not well separated from the unknown impurity at the position of 4.688min, which affects the detection result.

Comparative Example 2

Take the standard solution and the solution to be tested in Example 3 as the detection object.

(1) A high performance liquid chromatograph is used, the chromatographic column is a C18 reversed-phase chromatographic column, the column length of the chromatographic column is 150 mm, the inner diameter of the column is 4.6 mm, and the column particle size is 5 μm; the temperature of the chromatographic column is 40 ° C; the mobile phase is acetonitrile In the mixed system with water, the volume ratio of acetonitrile to water was 35:65; the sample volume for each injection was 5 μL, the flow rate of the mobile phase was 1 mL/min; the detection wavelength was set to 254 nm.

(2) After the baseline of the instrument is stable, inject the samples in the order of the standard, the sample to be tested, the standard product, and the sample to be tested, and calculate the (E)-2-(2-bromomethyl) of the standard solution and the sample solution to be tested, respectively. Phenyl)-2-methoxyimino methyl acetate peak area average, detection data as shown in Table 5 below:

Table 5 test results of comparative example 2

(3) calculate the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the sample to be tested according to the formula of external standard method, and the specific formula is the same as that in Example 1 , the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the sample to be tested is calculated to be 45.50%.

FIG. 9 and FIG. 10 are the chromatograms of the standard product and the sample to be tested in this embodiment, respectively. In Figure 9, the peak corresponding to the 14.332min position represents (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester, and the peak corresponding to the 19.921min position represents (E)-2 -(2-Dibromomethylphenyl)-2-methoxyiminoacetic acid methyl ester impurity; in Figure 10, the peak corresponding to the 14.400min position represents (E)-2-(2-bromomethylphenyl) -Methyl 2-methoxyiminoacetate, the corresponding peak at 19.294min represents (E)-2-(2-dibromomethylphenyl)-methyl 2-methoxyiminoacetate impurity, 20.829min The peak corresponding to the position represents the Z isomer. Using the conditions of this comparative example, although the detection result has no great influence, the retention time is later and the analysis period is long.

Test Example 1 Stability Test

Take the sample solution to be tested in the embodiment 1 as the investigation object, adopt high performance liquid chromatograph with diode array detector, analyze once at regular intervals at room temperature, analyze 6 times in total, and record the peak area simultaneously, the analysis conditions are the same as the implementation example 1.

The results are shown in Table 6 below, and the RSD is less than 1% by comparing the peak areas, indicating that the analytical method described in the present invention has good stability.

Table 6 Stability test results

Test Example 2 Precision Test

Take the (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester of Example 2 small test sample 20220215 batches as the investigation object, take standard product 0.0569g and five parallel The samples to be tested were injected in the order of standard solution, sample solution to be tested, standard solution and sample solution to be tested, and the (E)-2-(2-bromomethylphenyl) in five parallel samples to be tested was calculated. )-2-methoxyiminoacetic acid methyl ester mass fraction. The analysis conditions were the same as in Example 1.

The results are shown in Table 7 below, comparing the mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester, the RSD is less than 1%, indicating that the The analytical method has good precision.

Table 7 Precision test results

Test Example 3 Recovery Test

Get the (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester of the batch of 20220225 batches of embodiment 3 small test samples as the object of investigation, divide it into five parts, add different quality (E)-2-(2-Bromomethylphenyl)-2-methoxyiminoacetate methyl ester standard, prepared as known (E)-2-(2-bromomethylphenyl)-2 - The solution of methyl methoxyiminoacetate was detected by high performance liquid chromatography with diode array detector, and the recovery rate of standard addition was calculated. The analysis conditions were the same as in Example 1.

The results are shown in Table 8 below, the recovery rates are all between 98% and 102%, and the average recovery rate is 99.82%, indicating that the experimental recovery rate meets the requirements.

Table 8 Recovery test results

Test Example 4 Linear Test

A series of standard substances of different quality were weighed, placed in a 100 mL volumetric flask, dissolved in methanol and fixed to volume, and the relationship between the peak area and the solution concentration was investigated after injection. The analysis conditions were the same as those in Example 1.

The results are shown in Table 9 and Figure 11 below, and the correlation coefficient is 0.999, indicating that the analytical method provided by the present invention meets the requirements linearly.

Table 9 Linearity test results

serial number Weighing weight/g Standard solution concentration/g/L Peak Area 1 Peak area 2 Average peak area 1 0.0331 0.331 1996642 1996923 1996782.5 2 0.0450 0.450 2711046 2723019 2717032.5 3 0.0561 0.561 3374826 3377014 3375920 4 0.0647 0.647 3907463 3907698 3907580.5 5 0.0741 0.741 4419042 4439336 4429189

It can be known from the above-mentioned test examples 1-4 that the analytical method for the content of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester provided by the present invention has high accuracy and is operable. It has good properties and can be widely used in the analysis and detection of the content of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester.

Although the present invention has been described in detail in conjunction with the preferred embodiments with reference to the accompanying drawings, the present invention is not limited thereto. Without departing from the spirit and essence of the present invention, those of ordinary skill in the art can make various equivalent modifications or substitutions to the embodiments of the present invention, and these modifications or substitutions should all fall within the scope of the present invention/any Those skilled in the art can easily think of changes or substitutions within the technical scope disclosed by the present invention, which should be included within the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope described in the claims.

Claims (8)

1. an analytical method of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester content, is characterized in that, adopts high performance liquid chromatography to analyze, including following step: (1) Dissolve the standard and the sample to be tested with methanol as a solvent to prepare the standard solution and the solution of the sample to be tested; (2) The detection wavelength is set within the range of 230-270 nm, and after the baseline of the instrument is stable, the samples are injected and analyzed in the order of standard product, sample to be tested, standard product, and sample to be tested. Among them, the chromatographic conditions include: the chromatographic column is C18 A reversed-phase chromatographic column, the column temperature is 30-50°C, the mobile phase is a mixed system of acetonitrile and 0.8% glacial acetic acid aqueous solution, and the volume ratio of acetonitrile and glacial acetic acid aqueous solution is 40-60:60-40; (3) Calculate the peak area average value of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the standard solution and the sample solution to be tested, and treat according to the formula of the external standard method The mass fraction of (E)-2-(2-bromomethylphenyl)-2-methoxyiminoacetic acid methyl ester in the test sample was calculated. 2 . The analysis method according to claim 1 , wherein the column length of the chromatographic column is 150 mm, the inner diameter of the column is 4.6 mm, and the particle size of the column is 5 μm. 3 . 3. The analysis method according to claim 1, wherein the temperature of the chromatographic column is 40°C. 4 . The analysis method according to claim 1 , wherein the detection wavelength of high performance liquid chromatography is set to 254 nm. 5 . 5. analysis method as claimed in claim 1 is characterized in that, the volume ratio of acetonitrile and glacial acetic acid aqueous solution is 50:50. 6 . The analysis method according to claim 1 , wherein the HPLC conditions further comprise: the sample volume for each injection is 5 μL. 7 . 7 . The analysis method according to claim 1 , wherein the HPLC conditions further comprise: the flow rate of the mobile phase is 0.8-1.2 mL/min. 8 . 8. The analysis method according to claim 7, wherein the flow rate of the mobile phase is 1.0 mL/min.

Images