CN114813999A - HPLC analysis method and application of xanthenone related substances - Google Patents
HPLC analysis method and application of xanthenone related substances Download PDFInfo
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- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
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- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
- G01N2030/342—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient fluid composition fixed during analysis
Abstract
The application relates to the technical field of xanthone analysis methods, and particularly discloses an HPLC (high performance liquid chromatography) analysis method and application of xanthone related substances. The HPLC analysis method comprises the following steps: preparing a sample solution, setting parameters and carrying out HPLC detection; the chromatographic column used for HPLC detection is a chromatographic column of octadecyl bonded silica gel filler; the xanthone related substance is 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one; and the application of the HPLC analysis method of the xanthone related substances in the aspect of pesticide raw pesticide detection. The HPLC analysis method for the xanthone related substances can be used for rapidly and accurately analyzing and determining the 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-one, and has the advantages of simplicity in operation, high sensitivity, high accuracy and the like.
Description
Technical Field
The application relates to the technical field of xanthone analysis methods, in particular to an HPLC analysis method and application of xanthone related substances.
Background
Mesotrione, also known as misetone, is an effective inhibitor of HPPD (4-hydroxyphenyl pyruvate dioxygenase), can yellow plant tissues and generate withered spots, further promotes the death of plants, and is often used as a technical pesticide in corn herbicides. When the mesotrione is used as the herbicide to weed corn fields, the mesotrione is harmless to the environment, has strong weeding effect, does not cause adverse effect on corn plants, and is the corn field herbicide with excellent service performance.
It has been found that mesotrione produces an impurity during its manufacture, namely 1-cyano-6- (methylsulfonyl) -7-nitro-9H-xanthen-9-one, which is a xanthone species that has been analyzed to be toxic. According to the requirement of the European Union standard, when mesotrione is used as the raw pesticide, the proportion of the impurities in the raw pesticide should be minimized, otherwise serious harm is caused to the environment and human body. In recent years, China also pays attention to impurity components in pesticide raw materials, and in registration of pesticide raw materials, registration enterprises are required to provide more than 0.1% of impurity conditions including impurity names, contents, structures, necessary qualitative spectrograms and the like. Therefore, the rapid and accurate qualitative analysis of the 1-cyano-6- (methylsulfonyl) -7-nitro-9H-xanthen-9-one is an essential detection link.
Disclosure of Invention
In order to qualitatively separate and measure 1-cyano-6- (methylsulfonyl) -7-nitro-9H-xanthene-9-ketone rapidly and accurately and obtain an excellent detection spectrogram, the application provides an HPLC analysis method and application of a xanthene ketone related substance.
In a first aspect, the present application provides a method for HPLC analysis of a xanthone-related substance, which employs the following technical scheme:
a method for HPLC analysis of a xanthone-related substance, comprising the steps of: preparing a sample solution, setting parameters and carrying out HPLC detection; the chromatographic column used for HPLC detection is an octadecyl bonded silica gel filler chromatographic column;
the xanthone related substance is 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-ketone, and the structure of the xanthone related substance is as follows:
the application provides an HPLC analysis method of xanthone related substances, which adopts a chromatographic column with octadecyl bonded silica gel packing, and realizes the rapid and accurate analysis and determination of 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-ketone through the steps of sample solution preparation, parameter setting, HPLC detection and the like.
Preferably, the HPLC detection adopts a mobile phase gradient elution method to separate the sample solution; the mobile phase gradient elution method comprises the following steps: at 0min, the mobile phase A is 40%, and the mobile phase B is 60%; the mobile phase A is linearly increased to 40-100% and the mobile phase B is linearly decreased to 60-0% in 0-10 min; 10-16min, the mobile phase A is 100%, and the mobile phase B is 0%; mobile phase a and mobile phase B are both in volume percent.
In the application, a mobile phase gradient elution method is adopted to analyze and measure 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-ketone, the polarity of the mobile phase is changed within a certain time, so that 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-ketone is eluted from a chromatographic column, and a detection spectrogram is obtained through ultraviolet spectrum. The gradient elution method has the advantages of short separation time, high detection sensitivity, good peak shape of the obtained spectrogram, proper peak height, intermediate peak-yielding position and the like.
Preferably, the mobile phase A is an organic phase; the mobile phase B is a buffer solution.
Further, the mobile phase B can be a sodium acetate solution or a potassium dihydrogen phosphate solution.
Preferably, the mobile phase a is acetonitrile; the mobile phase B is a sodium acetate solution.
The acetonitrile-sodium acetate solution or acetonitrile-potassium dihydrogen phosphate solution is used as a mobile phase, and the 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-ketone can be analyzed and determined quickly and accurately. The mobile phase has good compatibility with a detector, high detection sensitivity and high separation degree, and can also improve the peak shape of a spectrogram and prolong the retention time of a sample to be detected on a chromatographic column, so that the obtained spectrogram has proper peak height and good peak shape symmetry.
Preferably, the concentration of the sodium acetate solution is 8-12 mM.
In a particular embodiment, the concentration of the sodium acetate solution may be 8mM, 10mM or 12 mM.
In some specific embodiments, the concentration of the sodium acetate solution may also be 8-10mM or 10-12 mM.
Preferably, the pH of the sodium acetate solution is 4-6.
In a particular embodiment, the pH of the sodium acetate solution may be 4, 5 or 6.
In some specific embodiments, the pH of the sodium acetate solution may also be 4-5 or 5-6.
In the application, acetonitrile and a sodium acetate solution are selected as the mobile phase, and the concentration and the pH value of the sodium acetate solution are adjusted within the range, so that the mobile phase can drive a sample to move in a chromatographic column, and meanwhile, the mobile phase can improve the retention time of the sample on the chromatographic column and ensure higher column efficiency.
Preferably, the parameter comprises a flow rate of the mobile phase, the flow rate of the mobile phase being 0.8-1.2 mL/min.
In a particular embodiment, the flow rate of the mobile phase may be 0.8mL/min, 1mL/min, or 0.8 mL/min.
In some specific embodiments, the flow rate of the mobile phase may also be from 0.8 to 1mL/min or from 1 to 1.2 mL/min.
The flow rate of the mobile phase is controlled within the range, so that the retention time of the sample on the chromatographic column is optimal, the analysis time is short, the peak position of the obtained spectrogram is moderate, and the peak shape is good.
Preferably, in the step of preparing the sample solution, the concentration of the sample to be detected is 0.1 mg/mL.
Preferably, the parameters further comprise a sample volume, and the sample volume is 3-6 μ L.
In a specific embodiment, the sample size may be 3 μ L, 5 μ L, or 6 μ L.
In some specific embodiments, the sample size may also be 3-5. mu.L or 5-6. mu.L.
According to the method, the sample volume is controlled within the range under the condition that the concentration of a sample to be detected is 0.1mg/mL, and the spectrogram obtained through analysis and detection is appropriate in peak height and good in peak shape symmetry.
Preferably, the parameters further include a wavelength, and the wavelength is 200-220 nm.
In a specific embodiment, the wavelength is 210 nm.
Preferably, the parameters further comprise a column temperature, and the column temperature is 25-40 ℃.
In a specific embodiment, the column temperature is 30 ℃.
According to the method, relevant parameters detected by HPLC are set in the range, the 1-cyano-6- (methylsulfonyl) -7-nitro-9H-xanthene-9-one can be quickly and accurately analyzed and detected, and each peak in a chromatogram presented after detection has good symmetry, proper peak height and centered peak position.
Preferably, the chromatographic column of the octadecyl bonded silica gel filler is a Silgreen C18 chromatographic column with the specification of 250X 4.6mm and 5 μm.
The chromatographic column of the Silgreen C18 chromatographic column is an octadecyl-bonded chromatographic column with silica gel filler with the aperture of 120A degrees, has the advantages of high theoretical plate number, excellent separation performance, good reproducibility and the like, and can effectively separate and measure 1-cyano-6- (methylsulfonyl) -7-nitro-9H-xanthene-9-one.
In a second aspect, the application provides an application of the method for analyzing xanthone-related substances by HPLC in the detection of pesticide raw drugs.
The 1-cyano-6- (methylsulfonyl) -7-nitro-9H-xanthene-9-ketone in the application belongs to one impurity in the original pesticide, and according to the registration standard of the original pesticide in China, the name, the content and the qualitative spectrogram of more than 0.1% of the impurity are required to be provided for the registered original pesticide.
In summary, the present application has the following beneficial effects:
1. the application provides an HPLC analysis method of xanthone related substances, which utilizes a chromatographic column of octadecyl bonded silica gel packing and adopts a gradient elution method to separate and measure 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-ketone, and the method has the characteristics of simple operation, high sensitivity, strong accuracy and easy standardized operation.
2. In the HPLC analysis method for the xanthone-related substances, a mixed solution of acetonitrile and a sodium acetate solution is used as a mobile phase, so that the retention time of the substances on a chromatographic column is prolonged, and 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-one can be quickly and accurately separated.
3. The application adopts an HPLC analysis method to separate 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-ketone, and obtains a detection spectrogram by scanning an ultraviolet spectrogram. In the HPLC analysis method, the symmetry of each peak in the chromatogram presented by scanning is good, the peak height is proper, the peak position is centered, and the separation effect is good by controlling the relevant parameters of HPLC detection.
4. The method provided by the application can be used for simply, quickly and accurately separating and measuring the 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one, and provides a high-quality impurity qualitative spectrogram for the original pesticide, so that the registration standard of the original pesticide is met.
Drawings
FIG. 1 is a flow chart of the HPLC analytical method detection of 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one provided herein.
FIG. 2 is a detection spectrum obtained by the HPLC analysis method of 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one provided in example 3.
Detailed Description
The application provides an HPLC analysis method of a xanthone-related substance, wherein the xanthone-related substance is 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-one, and the structure of the xanthone-related substance is as follows:
the HPLC analysis method of 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one, as shown in FIG. 1, specifically comprises the following steps:
(1) and dissolving a sample to be detected by using acetonitrile to prepare a sample solution with the concentration of 0.1-0.3 mg/mL.
(2) The parameters in the liquid chromatograph are set as follows: the temperature of the chromatographic column is 25-40 ℃; the sample injection amount is 3-6 mu L; the detection wavelength is 200-220 nm; the flow rate of the mobile phase is 0.8-1.2 mL/min.
(3) Then injecting the sample solution prepared in the step (1) into a liquid chromatograph, and separating the sample solution by adopting a mobile phase gradient elution method; the chromatographic column used is a Silgreen C18 chromatographic column bonded with octadecyl and silica gel filler with the aperture of 120A degrees, the specification is 250 multiplied by 4.6mm, and the size is 5 mu m.
The mobile phase gradient elution method comprises the following steps: at 0min, the mobile phase A is 40%, and the mobile phase B is 60%; the mobile phase A is linearly increased to 40-100% and the mobile phase B is linearly decreased to 60-0% in 0-10 min; 10-16min, the mobile phase A is 100%, and the mobile phase B is 0%; mobile phase a and mobile phase B are both in volume percent.
The mobile phase A is an organic phase; the mobile phase B is a buffer solution. Further, the mobile phase A is acetonitrile; the mobile phase B is a sodium acetate solution. The concentration of the sodium acetate solution is 8-12 mM; the pH value of the sodium acetate solution is 4-6.
The Silgreen C18 chromatographic column is purchased from Beijing Baicao scientific development Co., Ltd; the remaining raw materials, reagents, solvents, etc. are commercially available.
The present application will be described in further detail with reference to examples, comparative examples and the accompanying drawings.
Examples
Examples 1 to 5
Examples 1-5 each provide a method for HPLC analysis of a xanthenone related substance. The xanthone related substance is 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one
The above embodiments differ in that: the concentration of sodium acetate solution in the mobile phase; specifically, the results are shown in Table 1.
The specific steps of the above embodiment are as follows:
(1) and dissolving a sample to be detected by using acetonitrile to prepare a sample solution with the concentration of 0.1 mg/mL.
(2) The parameters of the liquid chromatograph are set as follows: the temperature of the chromatographic column is 30 ℃; the sample injection amount is 5 mu L; the detected wavelength is 210 nm; the flow rate of the mobile phase was 1 mL/min.
(3) Then injecting the sample solution prepared in the step (1) into a liquid chromatograph, and separating the sample solution by adopting a mobile phase gradient elution method; the chromatographic column used is a Silgreen C18 chromatographic column bonded with octadecyl and silica gel filler with the aperture of 120A degrees, the specification is 250 multiplied by 4.6mm, and the size is 5 mu m.
The mobile phase gradient elution method comprises the following steps: at 0min, acetonitrile is 40%, and sodium acetate solution is 60%; linearly increasing acetonitrile to 40-100% and linearly decreasing sodium acetate solution to 60-0% in 0-10 min; 10-16min, acetonitrile 100%, sodium acetate solution 0%; acetonitrile and sodium acetate solution are calculated according to volume percentage; wherein the sodium acetate solution has a concentration of 10mM and a pH of 5.
Table 1 concentration of sodium acetate solution in HPLC analytical methods provided in examples 1-5
Examples 6 to 9
Examples 6-9 each provide a method for HPLC analysis of a xanthenone related substance.
The above embodiment is different from embodiment 3 in that: the pH of the sodium acetate solution in the mobile phase; specifically, as shown in table 2.
Table 2 pH of sodium acetate solution in HPLC analytical methods provided in example 3, examples 6-9
| Examples | pH of sodium acetate solution |
| 3 | 5 |
| 6 | 3 |
| 7 | 4 |
| 8 | 6 |
| 9 | 7 |
Examples 10 to 13
Examples 10-13 each provide a method for HPLC analysis of xanthone-related substances.
The above embodiment is different from embodiment 3 in that: the flow rate of the mobile phase; specifically, the results are shown in Table 3.
Table 3 flow rates of mobile phases in HPLC analysis methods provided in example 3, examples 10-13
Examples 14 to 17
Examples 14-17 each provide a method for HPLC analysis of a xanthenone related substance.
The above embodiment is different from embodiment 3 in that: the sample introduction amount of the sample; the details are shown in Table 4.
Table 4 sample loading for HPLC analytical methods provided in example 3 and examples 14-17
| Examples | Sample volume (μ L) |
| 3 | 5 |
| 14 | 1 |
| 15 | 3 |
| 16 | 6 |
| 17 | 8 |
Example 18
Example 18 provides a method for HPLC analysis of xanthone-related substances.
The above embodiment is different from embodiment 3 in that: the mobile phase B is potassium dihydrogen phosphate solution.
Comparative example
Comparative example 1
Comparative example 1 provides a method for HPLC analysis of xanthenone related substances.
The above comparative example differs from example 3 in that: the mobile phase A is methanol.
Comparative example 2
Comparative example 2 provides a method for HPLC analysis of xanthenone related substances.
The above comparative example differs from example 3 in that: the chromatographic column used for separation and identification is a Symmetry C8(MOS) chromatographic column.
The result of the detection
1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one was separated and measured by the HPLC analysis method for xanthone-related substances provided in examples 1 to 18 and comparative examples 1 to 2, and an analysis spectrum was obtained by UV spectroscopy, and the analysis spectrum was as shown in FIG. 5:
TABLE 5 analysis spectra obtained in examples 1 to 18 and comparative examples 1 to 2
As can be seen from the results of the spectrum analyses obtained in examples 1 to 18 and comparative example 2 in Table 5, the method using Silgreen C18 column provided in examples 1 to 18 can be used to separately measure 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one; the spectrum obtained by separating and measuring 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one by using Symmetry C8(MOS) chromatographic column provided by the comparative example 2 has poor separation degree, poor peak shape and left peak position, so that the method is not suitable for separating and measuring 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one. Therefore, the chromatographic column adopting the octadecyl bonded silica gel filler can effectively separate and measure the 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-ketone, and has good separation effect and high detection speed.
As can be seen from the analysis spectrograms obtained in the comparative examples 1 to 5, the spectrograms obtained by the HPLC analysis method with the sodium acetate solution concentration of 8 to 12mM provided in the examples 2 to 4 have proper peak height, good peak shape symmetry, intermediate peak emergence positions and proper separation time; the HPLC analysis method with the sodium acetate solution concentration of 5mM provided in example 1 has a suitable peak height, but has a poor peak shape, a right peak position and a long separation time; although the chromatogram obtained by the HPLC analysis method with the sodium acetate solution concentration of 15mM provided in example 5 has a proper peak height, a fast separation speed and good symmetry of peak shape, the position of the peak is left, and when the sodium acetate solution concentration is greater than 15mM, the liquid phase detection system is easily blocked, which causes instrument damage. Therefore, the concentration of the sodium acetate solution is controlled within the range of 8-12mM, so that the 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-ketone can be quickly and accurately separated, and the obtained analysis spectrogram has proper peak height, good peak shape and centered peak emergence position. Fig. 2 shows a detection spectrum obtained by the HPLC analysis method of 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one provided in example 3.
By comparing the analytical spectrograms obtained in examples 6 to 9, it can be seen that the peak shapes of the spectrograms obtained gradually worsen and the peak positions gradually move toward the middle as the pH of the sodium acetate solution increases; and when the pH value of the sodium acetate solution is more than 6, the spectrogram has obvious tailing phenomenon. Therefore, the pH value of the sodium acetate solution is controlled within the range of 4-6, the 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-ketone can be separated and measured quickly and accurately, and the obtained spectrogram has the advantages of proper peak height, good peak shape symmetry and centered peak emergence position.
As can be seen from the analysis spectrograms obtained in examples 10 to 13, as the flow rate of the mobile phase increases, the symmetry of the obtained analysis spectrograms gradually deteriorates, the peak position moves leftward, and the separation time gradually increases; further comparison shows that the comprehensive effects of the peak shape, the peak position and the separation time of the spectrograms obtained in examples 11 to 12 are better than the comprehensive effects of the peak shape, the peak position and the separation time of the spectrograms obtained in examples 10 and 13. Therefore, the flow rate of the mobile phase is controlled within the range of 0.8-1.2mL/min, and an HPLC analysis spectrogram with excellent comprehensive effect can be obtained.
Comparing the analysis spectra obtained in examples 14-17, wherein the peak heights of the analysis spectra gradually increased with the increase of the sample amount when the sample concentration was 0.1 mg/mL; further comparison shows that when the sample injection amount is less than 3 mu L, the absorption of a spectrogram is weak, the peak is too low, and the peak shape is poor; when the sample amount is more than 6. mu.L, the absorption of the spectrogram is too strong, the peak is too high, and the peak shape is poor. Therefore, when the sample concentration is 0.1mg/mL, the sample injection amount is set to be 3-6 mu L, and a spectrogram with proper peak height, good peak shape symmetry and centered peak position can be obtained.
Comparing the separation cases of example 3 and example 18, it is clear that both the method using acetonitrile as the mobile phase a and a sodium acetate solution as the mobile phase B provided in example 3 and the method using acetonitrile as the mobile phase a and a potassium dihydrogen phosphate solution as the mobile phase B provided in example 18 can sequentially elute 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one from a chromatographic column, thereby achieving effective separation and detection of 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one.
Comparing the separation cases of example 3, example 18 and comparative example 1, it can be seen that comparative example 1 provides a method for separating and measuring 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one by using methanol as mobile phase A, and the obtained spectrum base line and peak shape are poor, the peak position is deviated to the right, the analysis time is long, and therefore, the method is not suitable for separating and measuring 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one. Therefore, in the method provided by the application, the acetonitrile-sodium acetate solution or the acetonitrile-potassium dihydrogen phosphate solution is used as the mobile phase, the 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-ketone can be quickly and effectively separated, and the obtained spectrogram has proper peak height, good peak shape symmetry and centered peak emergence position.
In summary, the method for analyzing xanthone-related substances by HPLC provided by the present application can simply, rapidly and accurately separate and measure 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthen-9-one, and has the characteristics of simple operation, high sensitivity, strong accuracy and easy standardized operation. The spectrogram detected by the method has good peak shape symmetry, proper peak height and centered peak outlet position, and can provide a high-quality qualitative spectrogram for pesticide raw material registration so as to meet the pesticide raw material registration standard.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. An HPLC analysis method for a xanthone-related substance, comprising the steps of: preparing a sample solution, setting parameters and carrying out HPLC detection; the chromatographic column used for HPLC detection is an octadecyl bonded silica gel filler chromatographic column;
the xanthone related substance is 1-cyano-6-methylsulfonyl-7-nitro-9H-xanthene-9-ketone, and the structure of the xanthone related substance is as follows:
2. the method for HPLC analysis of a xanthone-related substance according to claim 1, wherein said HPLC detection employs a mobile phase gradient elution method for separating said sample solution;
the mobile phase gradient elution method comprises the following steps: at 0min, the mobile phase A is 40%, and the mobile phase B is 60%; the mobile phase A is linearly increased to 40-100% and the mobile phase B is linearly decreased to 60-0% in 0-10 min; 10-16min, the mobile phase A is 100%, and the mobile phase B is 0%; mobile phase a and mobile phase B are both in volume percent.
3. The method for HPLC analysis of a xanthone-related substance according to claim 2, wherein said mobile phase a is an organic phase; the mobile phase B is a buffer solution.
4. The method for HPLC analysis of a xanthone-related substance according to claim 2, wherein said mobile phase a is acetonitrile; the mobile phase B is a sodium acetate solution.
5. The method for HPLC analysis of a xanthone-related substance according to claim 4, wherein the concentration of said sodium acetate solution is 8 to 12 mM.
6. The method for HPLC analysis of a xanthenone related substance according to claim 4, wherein the pH of the sodium acetate solution is 4 to 6.
7. The method for HPLC analysis of a xanthone-related substance according to claim 1, wherein said parameters include a flow rate of the mobile phase, said flow rate of the mobile phase being 0.8-1.2 mL/min.
8. The method for HPLC analysis of a xanthenone related substance according to claim 1, wherein said parameters further comprise a sample amount, said sample amount being 3 to 6 μ L.
9. The method for HPLC analysis of a xanthone-related substance according to claim 1, wherein said octadecyl-bonded silica gel filler column is a Silgreen C18 column, 250 x 4.6mm in size, 5 μm in size.
10. Use of the method for HPLC analysis of a xanthenone related substance as claimed in any one of claims 1 to 9 for the detection of a technical pesticide.
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| CN101696963A (en) * | 2009-10-29 | 2010-04-21 | 安徽华星化工股份有限公司 | Method for analyzing liquid chromatogram of methyl sulcotrione |
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