CN114384172A - Emamectin benzoate purity detection method - Google Patents
Emamectin benzoate purity detection method Download PDFInfo
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- CN114384172A CN114384172A CN202111546475.7A CN202111546475A CN114384172A CN 114384172 A CN114384172 A CN 114384172A CN 202111546475 A CN202111546475 A CN 202111546475A CN 114384172 A CN114384172 A CN 114384172A
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- G01—MEASURING; TESTING
- 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
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Abstract
A method for detecting the purity of emamectin benzoate comprises the following steps: the method comprises the following steps: weighing 100mg of emamectin benzoate sample, dissolving the emamectin benzoate sample in methanol, and putting the solution into a 100ml volumetric flask for constant volume to obtain 1mg/ml emamectin benzoate solution; step two: sending the emamectin benzoate solution obtained in the step one into a liquid chromatograph for spectrum analysis, wherein the conditions of the liquid chromatograph are as follows: a chromatographic column: chromatographic column with octadecylsilane chemically bonded silica as filler; mobile phase: acetonitrile: ammonium acetate solution at a concentration of 0.1% ═ 58: 42; flow rate: gradient flow rate elution; detection wavelength: 244 nm; column temperature: 40 ℃; sample introduction amount: 10 μ l. The invention can efficiently separate the emamectin benzoate from the impurities through liquid phase detection, has high impurity separation degree, can effectively identify 17 impurities, can better and accurately know the quality of the emamectin benzoate product so as to control the quality and safety of the product, and can improve the problems existing in the process flow through the types and the amount of the impurities so as to reduce the impurities in the product and improve the product quality.
Description
Technical Field
The invention belongs to the field of emamectin benzoate detection, and particularly relates to an emamectin benzoate purity detection method.
Background
The emamectin benzoate is used as a pesticide raw material, and the existing detection method is used for effectively identifying 17 kinds of impurities, has high impurity separation identification degree and better controls the quality and safety of products.
Disclosure of Invention
The invention provides a method for detecting the purity of emamectin benzoate, which is used for overcoming the defects in the prior art.
The invention is realized by the following technical scheme:
a method for detecting the purity of emamectin benzoate comprises the following steps:
the method comprises the following steps: weighing 100mg of emamectin benzoate sample, dissolving the emamectin benzoate sample in methanol, and putting the solution into a 100ml volumetric flask for constant volume to obtain 1mg/ml emamectin benzoate solution;
step two: sending the emamectin benzoate solution obtained in the step one into a liquid chromatograph for spectrum analysis, wherein the conditions of the liquid chromatograph are as follows: a chromatographic column: chromatographic column with octadecylsilane chemically bonded silica as filler; mobile phase: acetonitrile: ammonium acetate solution at a concentration of 0.1% ═ 58: 42; flow rate: gradient flow rate elution; detection wavelength: 244 nm; column temperature: 40 ℃; sample introduction amount: 10 μ l.
In the above method for detecting the purity of emamectin benzoate, the methanol in the first step is chromatographically pure methanol.
In the above method for detecting the purity of emamectin benzoate, the acetonitrile in the second step is chromatographically pure acetonitrile.
In the above method for detecting the purity of emamectin benzoate, the gradient flow rate in the second step is as follows: the flow rate is 1.2ml/min for 0-25min, 1.7ml/min for 25-58min, and 1.2ml/min for 58-60 min.
The invention has the advantages that: the invention can efficiently separate the emamectin benzoate from the impurities through liquid phase detection, has high impurity separation degree, can effectively identify 17 impurities, can better and accurately know the quality of the emamectin benzoate product so as to control the quality and safety of the product, and can improve the problems existing in the process flow through the types and the amount of the impurities so as to reduce the impurities in the product and improve the product quality.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is one of the liquid chromatograms obtained in the present invention;
FIG. 2 is a second liquid chromatogram obtained according to the present invention;
FIG. 3 is a third liquid chromatogram obtained in the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for detecting the purity of emamectin benzoate comprises the following steps:
the method comprises the following steps: weighing 100mg of emamectin benzoate sample, dissolving the emamectin benzoate sample in methanol, and putting the solution into a 100ml volumetric flask for constant volume to obtain 1mg/ml emamectin benzoate solution;
step two: sending the emamectin benzoate solution obtained in the step one into a liquid chromatograph for spectrum analysis, wherein the conditions of the liquid chromatograph are as follows: a chromatographic column: chromatographic column with octadecylsilane chemically bonded silica as filler; mobile phase: acetonitrile: ammonium acetate solution at a concentration of 0.1% ═ 58: 42; flow rate: gradient flow rate elution; detection wavelength: 244 nm; column temperature: 40 ℃; sample introduction amount: 10 μ l.
Preferably, the methanol in the first step is chromatographically pure methanol.
Preferably, the acetonitrile in the second step is chromatographically pure acetonitrile.
Preferably, the flow rate of the gradient flow rate elution in the second step is as follows: the flow rate is 1.2ml/min for 0-25min, 1.7ml/min for 25-58min, and 1.2ml/min for 58-60 min.
As can be seen from FIGS. 1-3, the liquid chromatography detection method of the application can effectively and efficiently separate the main peaks and the impurity peaks of the emamectin benzoate to obtain the accurate purity of the emamectin benzoate, and the impurity peaks are well separated to facilitate the analysis of the substances of the impurities, so that the corresponding standard peaks can be obtained, more detailed product information can be provided for customers, problems which may occur in each batch of production operation can be judged according to the types of the impurities, and the problems can be improved in the subsequent operation to improve the quality of the subsequent products.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (4)
1. A emamectin benzoate purity detection method is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: weighing 100mg of emamectin benzoate sample, dissolving the emamectin benzoate sample in methanol, and putting the solution into a 100ml volumetric flask for constant volume to obtain 1mg/ml emamectin benzoate solution;
step two: sending the emamectin benzoate solution obtained in the step one into a liquid chromatograph for spectrum analysis, wherein the conditions of the liquid chromatograph are as follows: a chromatographic column: chromatographic column with octadecylsilane chemically bonded silica as filler; mobile phase: acetonitrile: ammonium acetate solution at a concentration of 0.1% ═ 58: 42; flow rate: gradient flow rate elution; detection wavelength: 244 nm; column temperature: 40 ℃; sample introduction amount: 10 μ l.
2. The emamectin benzoate purity detection method according to claim 1, which is characterized in that: the methanol in the step one is chromatographic pure methanol.
3. The emamectin benzoate purity detection method according to claim 1, which is characterized in that: and the acetonitrile in the second step is chromatographic pure acetonitrile.
4. The emamectin benzoate purity detection method according to claim 1, which is characterized in that: the flow rate of gradient flow rate elution in the second step is as follows: the flow rate is 1.2ml/min for 0-25min, 1.7ml/min for 25-58min, and 1.2ml/min for 58-60 min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111546475.7A CN114384172A (en) | 2021-12-16 | 2021-12-16 | Emamectin benzoate purity detection method |
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| CN202111546475.7A CN114384172A (en) | 2021-12-16 | 2021-12-16 | Emamectin benzoate purity detection method |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113341038A (en) * | 2021-05-14 | 2021-09-03 | 河北威远生物化工有限公司 | Method for measuring content of emamectin benzoate |
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- 2021-12-16 CN CN202111546475.7A patent/CN114384172A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113341038A (en) * | 2021-05-14 | 2021-09-03 | 河北威远生物化工有限公司 | Method for measuring content of emamectin benzoate |
Non-Patent Citations (4)
| Title |
|---|
| AIYALU RAJASEKARAN 等: "Analysis of Emamectin Benzoate Residues in Cauliflower using HPLC", 《RESEARCH J. PHARM. AND TECH.》, vol. 6, no. 10, pages 1157 - 1160 * |
| 张健希: "液相色谱-串联质谱法检测仙草中甲氨基阿维菌素苯甲酸盐的残留", 《质量安全与检验检测》, vol. 30, no. 4, pages 2 * |
| 梁振益 等: "反相液相色谱法测定甲氨基阿维菌素苯甲酸盐的含量", 《海南大学学报(自然科学版)》, vol. 24, no. 2, pages 115 - 118 * |
| 毕富春 等: "高效液相色谱法定量分析甲氨基阿维菌素苯甲酸盐", 《农药科学与管理》, vol. 24, no. 3, pages 3 - 2 * |
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