An analytical method for the content of 2,3-dimethyl-4-bromophenyl methyl sulfone

Abstract

The present invention relates to the technical field of chemical analysis, and particularly relates to an analytical method for the content of 2,3-dimethyl-4-bromophenyl sulfone. The specific method is as follows: (1) Use methanol as a solvent to prepare a standard solution and a sample solution to be measured. The concentration ranges of both the standard solution and the sample solution to be measured are 0.3 - 0.6 mg / mL; (2) Set the detection wavelength within 230 - 270 nm. After the instrument baseline is stable, inject samples in the order of standard, sample to be measured, sample to be measured, and standard in sequence, and calculate the average peak areas of 2,3-dimethyl-4-bromophenyl sulfone in the standard solution and the sample solution to be measured respectively; (3) Calculate the mass fraction X1 of 2,3-dimethyl-4-bromophenyl sulfone in the sample solution to be measured according to the external standard method formula. The present invention fills the technical gap, has strong specificity, good precision, high recovery rate, high credibility, and good repeatability, and is particularly suitable for the quality control of pesticide technical products.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical analysis, and specifically relates to an analytical method for the content of 2,3-dimethyl-4-bromophenyl sulfone. Background Art

[0002] Topramezone is a benzoyl pyrazolone herbicide developed by BASF. It belongs to the hydroxyphenylpyruvate dioxygenase (HPPD) inhibitor. Its common English name is topramezone, and its Chinese name is topramezone or benzobicyclon. It can effectively control annual gramineous weeds and broad-leaved weeds in corn fields, is safe for corn, and its scope of application has gradually expanded to crops such as rice and sugarcane. It can be safely compounded with other pesticides. Topramezone has excellent efficacy and broad market prospects.

[0003] 2,3-Dimethyl-4-bromophenyl sulfone is an intermediate for the synthesis of topramezone. At present, the analytical method for accurately detecting the content of 2,3-dimethyl-4-bromophenyl sulfone is still blank. Since its content accuracy directly affects the accuracy of its downstream products, and then affects the accuracy of the topramezone content, therefore, finding an analytical method for stably and accurately detecting the content of 2,3-dimethyl-4-bromophenyl sulfone has an important role and practical significance for ensuring the quality of topramezone products. Summary of the Invention

[0004] Aiming at the technical problem that the analytical method for accurately detecting the content of 2,3-dimethyl-4-bromophenyl sulfone is still blank at present, the present invention provides an analytical method for the content of 2,3-dimethyl-4-bromophenyl sulfone, which fills the technical blank, has strong specificity, good precision, high recovery rate, high credibility, good repeatability, and is particularly suitable for the quality control of pesticide technical products.

[0005] The technical solution of the present invention is as follows:

[0006] An analytical method for the content of 2,3-dimethyl-4-bromophenyl sulfone, adopting a high performance liquid chromatography analysis method. The specific method is as follows:

[0007] (1) Dissolve the standard product and the sample to be tested with methanol as the solvent respectively to prepare a standard product solution and a sample to be tested solution. The concentration ranges of the standard product solution and the sample to be tested solution are both 0.3 - 0.6 mg / mL;

[0008] (2) Set the detection wavelength of the high performance liquid chromatography within 230 - 270 nm. After the instrument baseline is stable, inject samples in the order of standard product, sample to be tested, sample to be tested, and standard product, and calculate the average peak area of 2,3-dimethyl-4-bromophenyl sulfone in the standard product solution and the sample to be tested solution respectively;

[0009] (3) Calculate the mass fraction X1 of 2,3-dimethyl-4-bromophenyl sulfone in the test sample solution according to the external standard method formula, and the specific formula is as follows:

[0010]

[0011] In the formula,

[0012] A1 - the average value of the peak area of 2,3-dimethyl-4-bromophenyl sulfone in the standard product solution,

[0013] A2 - the average value of the peak area of 2,3-dimethyl-4-bromophenyl sulfone in the test sample solution,

[0014] m1 - the mass of the standard product,

[0015] m2 - the mass of the test sample,

[0016] P1 - the mass fraction of 2,3-dimethyl-4-bromophenyl sulfone in the standard product;

[0017] Among them, the high performance liquid chromatography conditions include:

[0018] The chromatographic column is an ODS-C18 reversed-phase chromatographic column, the chromatographic column temperature is 30 - 50 °C, and the mobile phase is a mixed system of acetonitrile and 0.8% aqueous acetic acid solution. Through a large number of experiments, the inventor of the present invention found that in the selection of the mobile phase, the use of acetonitrile and 0.8% aqueous acetic acid solution can effectively separate the target substance from the impurities, and it is superior to other solvents in terms of economic applicability. Here, the 0.8% aqueous acetic acid solution means that the volume percentage of acetic acid in the solution is 0.8%.

[0019] Preferably, the detection wavelength of the high performance liquid chromatography is 254 nm.

[0020] Preferably, the column length of the chromatographic column is 150 mm, the column inner diameter is 4.5 - 5 mm, more preferably 4.6 mm, and the column particle size is 3.5 μm.

[0021] Preferably, the temperature of the chromatographic column is 40 °C.

[0022] Preferably, the volume fraction of the 0.8% aqueous acetic acid solution in the mobile phase is 20% - 50%, more preferably 45%.

[0023] Preferably, the high performance liquid chromatography conditions further include: the sample volume for each injection is 5 μL, and the flow rate of the mobile phase is 1 mL / min.

[0024] The beneficial effects of the present invention are as follows:

[0025] (1) The present invention uses high performance liquid chromatography to detect the content of 2,3-dimethyl-4-bromobenzenesulfone, including an ODS-C18 reversed-phase chromatographic column, a column temperature of 30-50 °C, a mobile phase of a mixed system of acetonitrile and 0.8% aqueous acetic acid solution, and a detection wavelength of 230-300 nm. It can accurately determine its content, filling the technical gap in the corresponding field of the prior art.

[0026] (2) Using the above method to detect the mass fraction of 2,3-dimethyl-4-bromobenzenesulfone is stable and accurate, improving the accuracy and stability of the detection. It can achieve complete separation of impurities and main peaks, with good chromatographic peak shapes, stable retention times, accurate integral calculation results, good repeatability, and high credibility of the obtained results. It is particularly suitable for the quality control of intermediate products of pesticide technicals and plays an important role and practical significance in ensuring the quality of the final product; at the same time, the obtained results are more accurate and timely, providing strong data support for the production of pinoxaden. Description of the Drawings

[0027] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, for those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0028] Figure 1 It is the chromatogram of the standard solution in Example 1.

[0029] Figure 2 It is the chromatogram of the sample solution to be measured in Example 1.

[0030] Figure 3 It is the chromatogram of the standard solution in Example 2.

[0031] Figure 4 It is the chromatogram of the sample solution to be measured in Example 2.

[0032] Figure 5 It is the chromatogram of the standard solution in Example 3.

[0033] Figure 6 It is the chromatogram of the sample solution to be measured in Example 3.

[0034] Figure 7 It is the linear relationship diagram in Test Example 4.

[0035] Figure 8 It is the linear relationship diagram with a wavelength of 275 nm in Comparative Example 1.

[0036] Figure 9 It is the linear relationship diagram with a wavelength of 280 nm in Comparative Example 1.

[0037] Among them, Figures 1-6 In the chromatogram of

[0038] Figures 7-9 In the linear relationship diagram of Specific implementation mode

[0039] In order to enable those skilled in the art to better understand the technical solutions in the present invention, the following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts shall fall within the protection scope of the present invention.

[0040] Example 1

[0041] In production, 122 batches were obtained, and 1780 kg of solid sample of 2,3-dimethyl-4-bromophenyl sulfone was obtained. The content of 2,3-dimethyl-4-bromophenyl sulfone in the product was analyzed. The method included the following steps:

[0042] (1) Accurately weigh 52.4 mg of 2,3-dimethyl-4-bromophenyl sulfone standard product and place it in a 100 mL volumetric flask. Add 90 mL of methanol, shake and dissolve it, and then dilute it to the scale with methanol to obtain a standard product solution for standby. The mass fraction P1 of 2,3-dimethyl-4-bromophenyl sulfone in the standard product is 97.4%;

[0043] Weigh 53.6 mg of the sample to be tested and place it in a 100 mL volumetric flask. Add 90 mL of methanol, shake and dissolve it, and then dilute it to the scale with methanol to obtain a sample solution to be tested for standby;

[0044] (2) Use a high performance liquid chromatograph. The chromatographic column is an ODS-C18 chromatographic column. The column length of the chromatographic column is 150 mm, the column inner diameter is 4.6 mm, and the column particle size is 3.5 μm; the temperature of the chromatographic column is 40 °C; the mobile phase is a mixed system of acetonitrile and 0.8% acetic acid aqueous solution. The volume fraction of 0.8% acetic acid aqueous solution in the mixed system is 45%; 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 at 254 nm;

[0045] (3) After the instrument baseline is stable, inject samples in the order of standard product, sample to be tested, sample to be tested, and standard product in sequence, and calculate the average value of the peak areas of 2,3-dimethyl-4-bromophenyl sulfone in the standard product solution and the sample solution to be tested respectively. The detection data are shown in Table 1 below.

[0046] Table 1 Detection results of Example 1

[0047]

[0048] (4) Calculate the mass fraction of 2,3-dimethyl-4-bromophenyl methyl sulfone in the sample to be tested according to the external standard method formula. The mass fraction of 2,3-dimethyl-4-bromophenyl methyl sulfone in the sample to be tested is calculated to be 98.6%.

[0049] The specific formula is as follows.

[0050]

[0051] In the formula,

[0052] A1—the average value of the peak area of 2,3-dimethyl-4-bromophenyl methyl sulfone in the standard solution;

[0053] A2—the average value of the peak area of 2,3-dimethyl-4-bromophenyl methyl sulfone in the sample solution to be tested;

[0054] m1—the mass of the standard product;

[0055] m2—the mass of the sample to be tested;

[0056] P1—the mass fraction of 2,3-dimethyl-4-bromophenyl methyl sulfone in the standard product;

[0057] X1—the mass fraction of 2,3-dimethyl-4-bromophenyl methyl sulfone in the sample to be tested.

[0058] Figure 1 This is the chromatogram of the standard solution in this example. The peak corresponding to the 10.331 min position in the figure is the characteristic peak of 2,3-dimethyl-4-bromophenyl methyl sulfone. Figure 2 This is the chromatogram of the sample solution to be tested measured in this example. The peak corresponding to the 10.298 min position is 2,3-dimethyl-4-bromophenyl methyl sulfone.

[0059] Example 2

[0060] For the small-scale sample batch 20220418, 88.9 g of solid was obtained. Analyze the content of 2,3-dimethyl-4-bromophenyl methyl sulfone in the product. The method includes the following steps:

[0061] (1) Accurately weigh 53.7 mg of 2,3-dimethyl-4-bromophenyl methyl sulfone standard product and place it in a 100 mL volumetric flask. Add 90 mL of methanol, shake and dissolve it, and then dilute it to the scale with methanol to obtain a standard solution for standby. The mass fraction P1 of 2,3-dimethyl-4-bromophenyl methyl sulfone in the standard product is 97.4%.

[0062] Accurately weigh 54.7 mg of the sample to be tested and place it in a 100 mL volumetric flask. Add 90 mL of methanol, shake to dissolve, and then dilute to the mark with methanol to obtain the sample solution to be tested for standby.

[0063] (2) Use a high-performance liquid chromatograph with an ODS-C18 reversed-phase chromatographic column. The column length of the chromatographic column is 150 mm, the column inner diameter is 4.6 mm, and the column particle size is 3.5 μm. The temperature of the chromatographic column is 40 °C. The mobile phase is a mixed system of acetonitrile and 0.8% acetic acid aqueous solution, and the volume fraction of the 0.8% acetic acid solution in the mixed system is 45%. 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 at 254 nm.

[0064] (3) After the instrument baseline is stable, inject samples in the order of standard sample, sample to be tested, sample to be tested, and standard sample, and calculate the average peak areas of the 2,3-dimethyl-4-bromophenyl sulfone in the standard sample solution and the sample to be tested solution respectively. The detection data are shown in Table 2 below.

[0065] Table 2 Detection Results of Example 2

[0066]

[0067] (4) Calculate the mass fraction of 2,3-dimethyl-4-bromophenyl sulfone in the sample solution to be tested according to the external standard method formula. The specific formula is the same as that in Example 1, and the calculated mass fraction of 2,3-dimethyl-4-bromophenyl sulfone in the sample solution to be tested is 98.8%.

[0068] Figure 3 is the chromatogram of the standard sample solution in this example. The peak corresponding to the position of 10.422 min in the figure is 2,3-dimethyl-4-bromophenyl sulfone. Figure 4 is the chromatogram of the sample solution to be tested in this example. The peak corresponding to the position of 10.440 min in the figure is 2,3-dimethyl-4-bromophenyl sulfone.

[0069] Example 3

[0070] In production, 105 batches were obtained, and 1740 kg of solid samples of 2,3-dimethyl-4-bromophenyl sulfone were obtained. The content of 2,3-dimethyl-4-bromophenyl sulfone in the product was analyzed. The method includes the following steps:

[0071] (1) Accurately weigh 53.5 mg of 2,3-dimethyl-4-bromophenyl sulfone standard sample and place it in a 100 mL volumetric flask. Add 90 mL of methanol, shake to dissolve, and then dilute to the mark with methanol to obtain the standard sample solution for standby. The mass fraction P1 of 2,3-dimethyl-4-bromophenyl sulfone in the standard sample is 97.4%.

[0072] Accurately weigh 54.1 mg of the sample to be tested and place it in a 100 mL volumetric flask. Add 90 mL of methanol, shake to dissolve, and then dilute to the mark with methanol to obtain the sample solution to be tested for standby.

[0073] (2) Use a high-performance liquid chromatograph equipped with a diode array detector. The chromatographic column is an ODS-C18 reversed-phase chromatographic column with a column length of 150 mm, an inner column diameter of 4.6 mm, and a column particle size of 3.5 μm. The temperature of the chromatographic column is 40 °C. The mobile phase is a mixed system of acetonitrile and 0.8% aqueous acetic acid solution, and the volume fraction of 0.8% aqueous acetic acid solution in the mixed system is 45%. 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 at 254 nm.

[0074] (3) After the instrument baseline is stable, inject samples in the order of standard sample, sample to be tested, standard sample, and sample to be tested. Calculate the average peak areas of the 2,3-dimethyl p-bromobenzenesulfone in the standard sample solution and the sample solution to be tested respectively. The detection data are shown in Table 3 below.

[0075] Table 3 Detection Results of Example 3

[0076]

[0077] (4) Calculate the mass fraction of 2,3-dimethyl p-bromobenzenesulfone in the sample to be tested according to the external standard method formula. The specific formula is the same as that in Example 1. The calculated mass fraction of 2,3-dimethyl p-bromobenzenesulfone in the sample to be tested is 98.4%.

[0078] Figure 5 is the chromatogram of the standard sample solution in this example. The peak corresponding to the position of 10.431 min in the figure is 2,3-dimethyl p-bromobenzenesulfone. Figure 6 is the chromatogram of the sample solution to be tested in this example. The peak corresponding to the position of 10.451 min in the figure is 2,3-dimethyl p-bromobenzenesulfone.

[0079] Test Example 1 Stability Test

[0080] Take the standard sample solution in Example 1 as the object of investigation, analyze it at room temperature at regular intervals, analyze it 5 times in total, and record the peak area at the same time.

[0081] The analysis conditions include: using a high-performance liquid chromatograph with a diode array detector, the chromatographic column is an ODS-C18 reversed-phase chromatographic column, the column length of the chromatographic column is 150 mm, the column inner diameter is 4.6 mm, and the column particle size is 3.5 μm; the temperature of the chromatographic column is 40 °C; the mobile phase is a mixed system of acetonitrile and an aqueous solution of 0.8% glacial acetic acid, and the volume fraction of the aqueous solution of 0.8% glacial acetic acid in the mixed system is 45%; the sample volume for each injection is 5 μL, the flow rate of the mobile phase is 1 mL / min, and the detection wavelength is 254 nm.

[0082] The results are shown in Table 4 below. The retention time of the chromatographic peak is stable. By comparing the peak areas, the RSD is less than 1%, indicating that the analysis method described in the present invention has good stability.

[0083] Table 4 Results of the stability test

[0084]

[0085] Test Example 2 Precision test

[0086] Taking the 2,3-dimethyl-4-bromophenyl sulfone of the small-scale test sample batch 20220418 in Example 2 as the object of investigation, weighing the standard product and five parallel test samples, and injecting samples in the order of the standard product solution, the test sample solution, the test sample solution, and the standard product solution, and calculating the mass fraction of 2,3-dimethyl-4-bromophenyl sulfone in the five parallel test samples.

[0087] The analysis conditions are: using a Shimadzu liquid chromatograph with a high-performance liquid chromatograph and a diode array detector, the chromatographic column is an ODS-C18 reversed-phase chromatographic column, the column length of the chromatographic column is 150 mm, the column inner diameter is 4.6 mm, and the column particle size is 3.5 μm; the temperature of the chromatographic column is 40 °C; the mobile phase is a mixed system of acetonitrile and an aqueous solution of 0.8% glacial acetic acid, and the volume fraction of the aqueous solution of 0.8% glacial acetic acid in the mixed system is 45%; the sample volume for each injection is 5 μL, the flow rate of the mobile phase is 1 mL / min; the detection wavelength is set at 254 nm.

[0088] The results are shown in Table 5 below. By comparing the mass fractions of 2,3-dimethyl-4-bromophenyl sulfone, the RSD is less than 1%, indicating that the analysis method described in the present invention has good precision.

[0089] Table 5 Results of the precision test

[0090]

[0091] Test Example 3 Recovery test

[0092] Taking the pilot sample batch 20220418 of 2,3-dimethyl-4-bromophenyl sulfone in Example 2 as the object of investigation, standard samples and five pilot samples with different masses were weighed, and standard samples with different masses were added, and the recovery rate of the added standard samples was calculated by injection.

[0093] The analysis conditions were as follows: a high-performance liquid chromatograph equipped with a diode array detector was used, the chromatographic column was an ODS-C18 chiral chromatographic column, the column length of the chromatographic column was 150 mm, the column inner diameter was 4.6 mm, and the column particle size was 3.5 μm; the temperature of the chromatographic column was 40 °C; the mobile phase was a mixed system of acetonitrile and 0.8% acetic acid aqueous solution, and the volume fraction of 0.8% acetic acid aqueous solution in the mixed system was 45%, the sample volume for each injection was 5 μL, and the flow rate of the mobile phase was 1 mL / min; the detection wavelength of the high-performance liquid chromatography was set at 254 nm.

[0094] The results are shown in Table 6 below. The recovery rates were all between 98% and 102%, and the average recovery rate was 99.26%, indicating that the recovery rate of this experiment met the requirements.

[0095] Table 6 Results of the recovery rate test

[0096]

[0097] Test Example 4 Linear test

[0098] A series of standard samples with different masses were weighed and placed in a 100 mL volumetric flask, dissolved with methanol and made up to the mark, and the relationship between the peak area and the solution concentration was investigated after injection;

[0099] The analysis conditions included: a high-performance liquid chromatograph equipped with a diode array detector was used, the chromatographic column was an ODS-C18 reverse-phase chromatographic column, the column length of the chromatographic column was 150 mm, the column inner diameter was 4.6 mm, and the column particle size was 3.5 μm; the temperature of the chromatographic column was 40 °C; the mobile phase was a mixed system of acetonitrile and 0.8% acetic acid aqueous solution, and the volume fraction of 0.8% acetic acid aqueous solution in the mixed system was 45%; the sample volume for each injection was 5 μL, the flow rate of the mobile phase was 1 mL / min, and the detection wavelength was 254 nm.

[0100] The results are as shown in Table 7 and Figure 7 as follows. The correlation coefficient was 1, indicating that the linearity of the analytical method provided by the present invention met the requirements.

[0101] Table 7 Results of the linear test

[0102] Serial number Sample weight / g Standard solution concentration / (g / L) Peak area 1 Peak area 2 Average peak area 1 0.0322 0.322 577478 577554 577516 2 0.0424 0.424 763097 760218 761657.5 3 0.0536 0.536 957889 957968 957928.5 4 0.0571 0.571 1021612 1018721 1020166.5 5 0.061 0.61 1088747 1086304 1087525.5

[0103] As can be seen from the above Test Examples 1-4, the analysis method for the content of 2,3-dimethyl-p-bromophenyl sulfone provided by the present invention has high accuracy and good operability, and can be widely applied to the analysis and detection of the content of 2,3-dimethyl-p-bromophenyl sulfone.

[0104] Comparison of linear detection results at different detection wavelengths in Comparative Example 1

[0105] In Test Example 4, wavelengths of 275 nm and 280 nm were also selected as detection wavelengths for linear verification, and the results are shown in Tables 8-9. It was found through verification that under the conditions of wavelengths 275 nm and 280 nm, although the linear correlation coefficient R 2 value was also greater than 0.99, the intercept was very large (as shown in Figure 8 and Figure 9 ), so when using the single standard comparison method of the present invention for sample analysis under this condition, the error was relatively large.

[0106] Table 8 Linear test results at 275 nm

[0107] Serial number Mass / g Standard sample concentration / (g / L) Peak area 1 Peak area 2 Average peak area 1 0.0322 0.322 1018923 1019609 1019266 2 0.0424 0.424 1347841 1343765 1345803 3 0.0536 0.536 1727458 1725045 1726252 4 0.0571 0.571 1841470 1835779 1838625 5 0.061 0.61 1965828 1962109 1963969

[0108] Table 9 Linear test results at 280 nm

[0109] Serial number Mass / g Standard sample concentration / (g / L) Peak area 1 Peak area 2 Average peak area 1 0.0322 0.322 1006496 1007408 1006952 2 0.0424 0.424 1337353 1334057 1335705 3 0.0536 0.536 1718547 1717958 1718253 4 0.0571 0.571 1798477 1793531 1796004 5 0.061 0.61 1919723 1916597 1918160

[0110] Although the present invention has been described in detail by referring to the accompanying drawings and in combination with preferred embodiments, 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 be within the scope covered by the present invention / Any person skilled in the art within the technical scope disclosed by the present invention can easily think of changes or substitutions, which should all be covered within the protection scope of the present invention.

Claims

1. A method for analyzing the content of 2,3-dimethyl-4-bromophenyl methyl sulfone, characterized in that, The high performance liquid chromatography analysis method is adopted, and the specific method is as follows: (1) Use methanol as the solvent to dissolve the standard product and the sample to be tested respectively, and prepare the standard product solution and the sample to be tested solution. The concentration ranges of the standard product solution and the sample to be tested solution are both 0.3 - 0.6 mg / mL; (2) Set the detection wavelength of the high performance liquid chromatography within 230 - 270 nm. After the instrument baseline is stable, inject samples in the order of standard product, sample to be tested, sample to be tested, and standard product, and calculate the average peak areas of 2,3 - dimethyl - p - bromobenzene sulfone in the standard product solution and the sample to be tested solution respectively; (3) Calculate the mass fraction X1 of 2,3 - dimethyl - p - bromobenzene sulfone in the sample to be tested solution according to the external standard method formula. The specific formula is as follows: In the formula, A1 — the average peak area of 2,3 - dimethyl - p - bromobenzene sulfone in the standard product solution, A2 — the average peak area of 2,3 - dimethyl - p - bromobenzene sulfone in the sample to be tested solution, m1 — the mass of the standard product, m2 — the mass of the sample to be tested, P1 — the mass fraction of 2,3 - dimethyl - p - bromobenzene sulfone in the standard product; Among them, the high performance liquid chromatography conditions include: The chromatographic column is an ODS - C18 reversed - phase chromatographic column, the chromatographic 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 fraction of 0.8% glacial acetic acid aqueous solution in the mobile phase is 45%. The detection wavelength of the high performance liquid chromatography is 254 nm.

2. The analysis method according to claim 1, characterized in that, The column length of the chromatographic column is 150 mm, the column inner diameter is 4.5 - 5 mm, and the column particle size is 3.5 μm.

3. The analysis method according to claim 2, characterized in that, The column inner diameter is 4.6 mm.

4. The analysis method according to claim 1, characterized in that The temperature of the chromatographic column is 40 °C.

5. The analysis method according to claim 1, characterized in that, The high performance liquid chromatography conditions also include: the sample volume for each injection is 5 μL, and the flow rate of the mobile phase is 1 mL / min.

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