CN113156012A - Method for separating and detecting effective components in synergistic ether and pyrethrin - Google Patents
Method for separating and detecting effective components in synergistic ether and pyrethrin Download PDFInfo
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Abstract
The invention belongs to the technical field of chromatographic detection, and particularly relates to a method for separating and detecting effective components in synergistic ether and pyrethrin. The method selects a high performance liquid chromatograph, pretreats a sample, uses an Epic C18 chromatographic column, and uses a gradient method to separate and detect the sample under specific chromatographic conditions, so as to effectively separate effective components in the synergistic ether and the pyrethrin. And a better peak shape and satisfactory degree of separation are obtained.
Description
Technical Field
The invention belongs to the technical field of chromatographic detection, and particularly relates to a method for separating and detecting effective components in synergistic ether and pyrethrin
Background
The natural pyrethrin is an active component extracted from pyrethrum, and the product is mainly used as a sanitary pesticide. The pyrethrin preparation mainly contains pyrethrin, and the natural pyrethrin is a mixture of 6 insecticidal components, namely pyrethrin I, guayulin I, jasmine chrysanthemin I, pyrethrin II, guayulin II and jasmine chrysanthemin II.
Synergistic ether (PBO) has a chemical name of piperonyl butoxide, short for ENT-14250, and is colorless to pale yellow oily transparent liquid. Has a slight peculiar smell and a bitter taste. The synergistic ether is a good synergistic agent, and can raise the insecticidal activity of pyrethrin and several pyrethroids, rotenone and carbamate insecticides. It has obvious synergistic effect on pyrethroid insecticide, stable property and no harm to mammal. Therefore, it is often used in combination with natural pyrethrin.
In the prior art, the research on the pyrethrin chromatographic technique mostly focuses on the research on 6 effective components of pyrethrin, such as plum derivative, Liuyuling, and the courser. TLC has the characteristics of small quantity of samples, high speed and simple and convenient operation, is suitable for qualitative analysis of pyrethrin, preliminarily judges whether the sample contains effective components or not, and provides reliable tracking experiment parameters for column chromatography. As long as the chromatographic column and corresponding experimental conditions are properly selected, the GC method and the HPLC method can separate the active components of the pyrethrin in turn, in contrast, the gas chromatography is the classic method for the separation and analysis of the pyrethrin, while the liquid chromatography is increasingly applied with its own advantages, and various combined technologies are also increasingly applied as the liquid chromatography.
However, in practical application, when the natural pyrethrin and the synergistic ether are mixed for use, the peaks of the jasminum-synanthrin I and the pyrethrin I always overlap with the peak of the synergistic ether by gas chromatographic analysis, and how to separate the three peaks has important significance without influencing the appearance of the peaks of other effective components of the natural pyrethrin.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a method for separating and detecting effective components in synergistic ether and pyrethrin. The method can effectively separate six effective components of synergistic ether and pyrethrin.
In order to achieve the above purpose, the technical scheme provided by the invention is as follows:
a method for separating and detecting effective components in synergistic ether and pyrethrin comprises the following steps:
(1) dissolving the sample with petroleum ether, diluting with ethanol, mixing, filtering, and collecting the supernatant as the sample to be tested;
(2) selecting high performance liquid chromatography, taking methanol water solution as mobile phase, and performing separation detection by gradient method; wherein the system gradient of the mobile phase is within 0-27min, 52-80% methanol water solution (volume concentration) is used as the mobile phase, and 80% methanol water solution is used as the mobile phase within 27-65 min.
Preferably, in the step (1), the amount of the petroleum ether used is 5 to 10 times of the mass of the sample.
Preferably, in the step (1), the mass of the ethanol is 10-20 times of that of the sample.
Preferably, in step (1), the sample concentration is 0.05-0.15mg/ml ethanol.
Preferably, in step (1), the filtration is performed with a 0.22 μm filter.
Preferably, in step (2), the high performance liquid chromatography is a RIGOL HPLC (L-3000) system;
preferably, in step (2), the column is an Epic C185 μm, 250X 4.6mm (Oriental Lankeei ES column);
preferably, in step (2), the chromatographic conditions are: mobile phase a/B (methanol/water); the column temperature is 30-40 ℃; the flow rate is 1.0-1.5 ml/min; the detection wavelength is UV 220-230 nm.
Preferably, in step (2), the gradient method is: within 0-10min, 52-60% methanol aqueous solution is used as mobile phase, within 10-16min, 60-72% methanol aqueous solution is used as mobile phase, within 16-27min, 72-75% methanol aqueous solution is used as mobile phase, within 27-65min, 75-80% methanol aqueous solution is used as mobile phase.
Preferably, in step (2), the gradient method is: running with 55% methanol water solution as mobile phase within 0-8min, running with 60% methanol water solution as mobile phase within 8-10min, running with 72% methanol water solution for 10-16min, running with 75% methanol water solution as mobile phase within 16-27min, and running with 80% methanol water solution as mobile phase within 27-65 min.
Preferably, the chromatographic conditions are such that the sample volume is 2-10. mu.L.
Compared with the prior art, the invention has the technical advantages that:
(1) the invention uses HPLC to successfully separate the synergistic ether from the pyrethrin I, the guayulin I, the jasmine chrysanthemin I, the pyrethrin II, the guayulin II and the jasmine chrysanthemin II for the first time, and obtains better peak shape and satisfactory separation degree.
(2) According to the method provided by the invention, the mobile phase component of HPLC analysis is simple, and no mobile phase additive is needed; the gradient method is less limited by instruments, is convenient to switch among the instruments, and prolongs the service life of the chromatographic column.
(3) The separation detection method provided by the invention has higher repeatability and stability.
(4) The invention performs HPLC separation on seven components, the separation degree reaches more than 1.5, the peak shape is better, and the components in the pyrethrin can be analyzed quickly and accurately. The HPLC analysis method is simple, easy to transfer among instruments and high in reproducibility.
Drawings
FIG. 1: chromatogram maps of standard samples of the components, wherein (a) is a standard chromatogram map of the guaifenesin II; (b) is a standard spectrogram of pyrethrin II; (c) is a standard spectrogram of the jasminum grandiflorum II; (d) standard spectrum of synergistic ether; (e) is a standard spectrogram of the guaifenesin I; (f) is a standard spectrogram of pyrethrin I; (g) is a standard spectrogram of the jasminum grandiflorum I;
FIG. 2: the chromatogram of example 1;
FIG. 3: the chromatogram of example 2;
FIG. 4: the chromatogram of example 3;
FIG. 5: the chromatogram of comparative example 1;
FIG. 6: the chromatogram of comparative example 2;
FIG. 7: the chromatogram of comparative example 3;
FIG. 8: the chromatogram of comparative example 4;
the specific meanings of the symbols in the drawings are as follows: 1: guapigenin II; 2: pyrethrin II; 3: heliotropin II; 4: a synergistic ether; 5: guarsaponin I; 6: pyrethrin I; 7: the jasmine chrysanthemin I.
The invention will now be further illustrated with reference to the accompanying drawings and examples:
Detailed Description
The present invention will be described below with reference to specific examples to make the technical aspects of the present invention easier to understand and grasp, but the present invention is not limited thereto. The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
The pyrethrin samples containing synergistic ethers used in the standard samples and examples and comparative examples of the present invention were obtained from yunnanbao biotechnology limited.
Example 1
A method for separating and detecting effective components in synergistic ether and pyrethrin comprises the following steps:
(1) dissolving a sample by adding 6 times of petroleum ether, adding ethanol to dilute the sample into 0.10mg/ml ethanol, uniformly mixing, filtering by using 0.22 mu m, and taking supernatant as a sample to be detected;
(2) selecting high performance liquid chromatography, taking methanol water solution as mobile phase, and performing separation detection by gradient method;
wherein: the high performance liquid chromatography is RIGOL HPLC (L-3000) system;
the column was an Epic C185 μm, 250X 4.6mm (Oriental Lankee ES column);
the chromatographic conditions are as follows: the column temperature is 30 ℃; the flow rate is 1.0 ml/min; the detection wavelength is UV 220-230 nm; the amount of sample was 2. mu.L.
The gradient method comprises the following steps: running with 55% methanol water solution as mobile phase within 0-8min, running with 60% methanol water solution as mobile phase within 8-10min, running with 72% methanol water solution for 10-16min, running with 75% methanol water solution as mobile phase within 16-27min, and running with 80% methanol water solution as mobile phase within 27-65 min.
Example 2
A method for separating and detecting effective components in synergistic ether and pyrethrin comprises the following steps:
(1) dissolving a sample by adding 5 times of petroleum ether, adding ethanol to dilute the sample into 0.15mg/ml ethanol, uniformly mixing, filtering by using 0.22 mu m, and taking supernatant as a sample to be detected;
(2) selecting high performance liquid chromatography, taking methanol water solution as mobile phase, and performing separation detection by gradient method; wherein: the high performance liquid chromatography is RIGOL HPLC (L-3000) system;
the column was an Epic C185 μm, 250X 4.6mm (Oriental Lankee ES column);
the chromatographic conditions are as follows: the column temperature was 40 ℃; the flow rate is 1.5 ml/min; the detection wavelength is UV 220-230 nm; the amount of sample was 10. mu.L.
The gradient method comprises the following steps: within 0-10min, 52% methanol aqueous solution is used as mobile phase, within 10-16min, 60% methanol aqueous solution is used as mobile phase, within 16-27min, 72% methanol aqueous solution is used as mobile phase, within 27-65min, 75% methanol aqueous solution is used as mobile phase.
Example 3
A method for separating and detecting effective components in synergistic ether and pyrethrin comprises the following steps:
(1) dissolving a sample by adding 10 times of petroleum ether, adding ethanol to dilute the sample into 0.05mg/ml ethanol, uniformly mixing, filtering by using 0.22 mu m, and taking supernatant as a sample to be detected;
(2) selecting high performance liquid chromatography, taking methanol water solution as mobile phase, and performing separation detection by gradient method; wherein: the high performance liquid chromatography is RIGOL HPLC (L-3000) system;
the column was an Epic C185 μm, 250X 4.6mm (Oriental Lankee ES column);
the chromatographic conditions are as follows: the column temperature was 35 ℃; the flow rate is 1.2 ml/min; the detection wavelength is UV 220-230 nm; the sample amount is 2-10 μ L.
The gradient method comprises the following steps: within 0-10min, 60% methanol water solution is used as mobile phase, within 10-16min 72% methanol water solution is used as mobile phase, within 16-27min 75% methanol water solution is used as mobile phase, within 27-65min 80% methanol water solution is used as mobile phase.
Comparative example 1
The only difference from example 1 is that the gradient method is different and the remaining operating steps are unchanged.
The gradient method of this example is: 0-27min, 45% methanol water solution; 27-65min, 72% methanol water solution.
Comparative example 2
The only difference from example 1 is that the gradient method is different and the remaining operating steps are unchanged.
The gradient method of this example is: 0-65 min, 75% methanol water solution.
Comparative example 3
The only difference from example 1 is that the mobile phase is different and the remaining operating steps are unchanged.
The gradient method comprises the following steps: running with 55% acetonitrile water solution as mobile phase within 0-8min, running with 60% acetonitrile water solution as mobile phase within 8-10min, running with 72% acetonitrile water solution within 10-16min, running with 75% acetonitrile water solution as mobile phase within 16-27min, and running with 80% acetonitrile water solution as mobile phase within 27-65 min.
Comparative example 4
The only difference from example 1 is that the rest of the operating steps are unchanged, unlike the column.
The column of this example is: caprisil C185 μm, 250X 4.6 mm.
Examples of effects
1. Chromatographic data
The qualitative analysis was carried out on the component standard samples (single standard samples) with reference to the conditions of example 1, while the same batch of samples was analyzed according to the methods described in examples 1 to 3 and comparative examples 1 to 4 above.
Wherein, the chromatogram of each component standard sample is shown in (a) - (g) in the figure 1, and the qualitative data is shown in the table 1.
The chromatographic data for examples 1-3 are shown in tables 2-4 and the chromatograms are shown in FIGS. 2-4.
The chromatograms of comparative examples 1-4 are shown in FIGS. 5-8.
TABLE 1 chromatographic data for single standard samples
| Component numbering | Composition (I) | Retention time/ |
| 1 | Gualoesin II | 32.061 |
| 2 | Pyrethrin II | 33.410 |
| 3 | Jasmine chrysanthemin II | 37.080 |
| 4 | Synergistic ethers | 39.220 |
| 5 | Gualoesin I | 45.817 |
| 6 | Pyrethrin I | 47.579 |
| 7 | Jasmine chrysanthemin I | 55.581 |
Table 2 chromatographic data for example 1
| Component numbering | Composition (I) | Retention time/min | Peak area | Column effect | Degree of separation | Symmetrical/ |
| 1 | Gualoesin II | 31.757 | 549.178 | 155780.585 | 1.006 | |
| 2 | Pyrethrin II | 33.533 | 4598.955 | 149898.901 | 2.361 | 1.012 |
| 3 | Jasmine chrysanthemin II | 37.117 | 332.153 | 108507.456 | 9.253 | 1.002 |
| 4 | Synergistic ethers | 39.160 | 6334.828 | 89874.368 | 4.313 | 1.048 |
| 5 | Gualoesin I | 45.730 | 614.791 | 71969.324 | 11.175 | 0.942 |
| 6 | Pyrethrin I | 47.101 | 7736.053 | 65996.755 | 1.979 | 1.004 |
| 7 | Jasmine chrysanthemin I | 55.420 | 446.412 | 55121.659 | 7.424 | 0.994 |
Table 3 chromatographic data for example 2
Table 4 chromatographic data for example 3
| Component numbering | Composition (I) | Retention time/min | Peak area | Column effect | Degree of separation | Symmetrical/ |
| 1 | Gualoesin II | 31.990 | 387.778 | 123893.065 | 0.920 | |
| 2 | Pyrethrin II | 32.750 | 1950.698 | 118189.640 | 2.042 | 0.921 |
| 3 | Jasmine chrysanthemin II | 37.383 | 106.082 | 96051.915 | 8.545 | 0.956 |
| 4 | Synergistic ethers | 39.223 | 2375.528 | 86872.631 | 3.724 | 0.926 |
| 5 | Gualoesin I | 45.890 | 422.764 | 66398.825 | 10.972 | 0.866 |
| 6 | Pyrethrin I | 47.197 | 3085.720 | 63478.224 | 1.828 | 0.911 |
| 7 | Jasmine chrysanthemin I | 55.497 | 145.841 | 50160.605 | 7.807 | 0.900 |
As can be seen from the data in tables 2-4, the analytical method provided by the invention can successfully separate the synergistic ether from the pyrethrin I, the guayulin I, the jasmine I, the pyrethrin II, the guayulin II and the jasmine II, and obtain better peak shape and satisfactory separation degree. From the data of comparative examples 1 to 4, it is understood that the above 7 components were not well separated or could not be detected when the conditions of mobile phase, chromatographic conditions, gradient method, etc. were changed.
2. Precision and stability experiments
Precision and stability experiments were performed as in example 1.
And (3) precision experiment: continuously feeding samples for 6 times by absorbing the solution of the reference substance, measuring the peak area of each reference substance, and calculating the relative standard deviation; the results are shown in Table 5.
Stability test: the peak area of each control was measured at 0 hour, 4 hours, 8 hours, 12 hours and 24 hours, respectively, and the results were as shown in Table 5 with respect to the standard deviation.
TABLE 5 precision and stability data
Therefore, the precision is 0.98-2.01%, the stability is 1.06-2.12%, and the method provided by the invention has high precision and good stability.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.
Claims (10)
1. A method for separating and detecting effective components in synergistic ether and pyrethrin comprises the following steps:
(1) dissolving the sample with petroleum ether, diluting with ethanol, mixing, filtering, and collecting the supernatant as the sample to be tested;
(2) selecting high performance liquid chromatography, taking methanol water solution as mobile phase, and performing separation detection by gradient method; wherein the system gradient of the mobile phase is within 0-27min, 52-80% methanol water solution is used as the mobile phase, and 80% methanol water solution is used as the mobile phase within 27-65 min.
2. The method for separating and detecting effective components in synergistic ether and pyrethrin according to claim 1, wherein in step (1), the amount of petroleum ether used is 5-10 times of the mass of the sample.
3. The method for separating and detecting active ingredients in synergistic ether and pyrethrin according to claim 1, wherein in step (1), the mass of said ethanol is 10-20 times of the mass of the sample.
4. The method of claim 1, wherein in step (1), the sample concentration is 0.05-0.15mg/ml ethanol.
5. The method of claim 1, wherein the effective components of the synergistic ether and pyrethrin are detected,
in the step (2), the high performance liquid chromatography is a RIGOL HPLC (L-3000) system.
6. The method of claim 1, wherein in step (2), the chromatographic column is Epic C185 μm, 250 x 4.6 mm.
7. The method for separating and detecting effective components in synergistic ether and pyrethrin according to claim 1, wherein in step (2), said chromatographic conditions are: mobile phase a/B (methanol/water); the column temperature is 30-40 ℃; the flow rate is 1.0-1.5 ml/min; the detection wavelength is UV 220-230 nm.
8. The method of claim 7, wherein the chromatographic conditions are carried out in an amount of 2 to 10 μ L.
9. The method for separating and detecting effective components in synergistic ether and pyrethrin according to claim 1, wherein in step (2), said gradient method is: within 0-10min, 52-60% methanol aqueous solution is used as mobile phase, within 10-16min, 60-72% methanol aqueous solution is used as mobile phase, within 16-27min, 72-75% methanol aqueous solution is used as mobile phase, within 27-65min, 75-80% methanol aqueous solution is used as mobile phase.
10. The method for separating and detecting effective components in synergistic ether and pyrethrin according to claim 1, wherein in step (2), said gradient method is: running with 55% methanol water solution as mobile phase within 0-8min, running with 60% methanol water solution as mobile phase within 8-10min, running with 72% methanol water solution for 10-16min, running with 75% methanol water solution as mobile phase within 16-27min, and running with 80% methanol water solution as mobile phase within 27-65 min.
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Application publication date: 20210723 |