Separation method and application of pesticide active substances in waste lavender straw

Abstract

The invention discloses a separation method and application of pesticide active substances from lavender waste straw, and relates to the technical field of separation of pesticide active substances, and the separation method specifically comprises the following separation steps: step 1, pretreatment: washing 120-170g of lavender waste straw, and then successively carrying out crushing, grinding and sieving treatment; step 2, extraction: adding a solvent into the treated lavender waste straws, and performing ultrasonic treatment on the treated lavender waste straws by adopting an ultrasonic instrument. According to the separation method and the application of the pesticide active substances in the waste lavender straw, the ethanol solution is adopted for filtering twice, so that some larger impurity particles can be removed through first-time filtering, and tiny impurities possibly remaining in the ethanol solution are further removed through second-time filtering on the basis of primary purification, so that the separation efficiency of the pesticide active substances in the waste lavender straw is improved. Samples can be effectively purified, so that the purity of pesticide active substances is improved; and two times of filtration are beneficial to precise separation of target pesticide active substances.

Description

Technical Field

[0001] The invention relates to the technical field of separation of pesticide active substances, and in particular to a method for separating pesticide active substances from waste lavender straw and application thereof. Background Art

[0002] Lavender waste straw contains a variety of substances with pesticide activity; the main ones are lavender essential oil components, such as linalool, linalyl acetate, etc. These components have antibacterial and insect repellent effects; for example, linalool can inhibit the growth of a variety of bacteria and fungi, and can prevent crops from being infected by microbial pathogens to a certain extent; linalyl acetate has a repellent effect on pests such as mosquitoes and mites, which can reduce the harm of pests to crops. However, the existing resource utilization of lavender waste straw is not high, and the methods for exploring and utilizing it in agricultural medicine are insufficient. Other similar methods are often used for reference, but in the process of separation and extraction of targeted pesticide active substances, usually only one filtration and one purification step are performed, resulting in a low purity of the separated pesticide active substances; for this reason, the present invention provides a separation method and application of pesticide active substances from lavender waste straw to solve the above-mentioned problems. Summary of the invention

[0003] In view of the deficiencies in the prior art, the present invention provides a method for separating pesticide active substances from waste lavender straw and its application, which solves the problems mentioned in the above background technology.

[0004] To achieve the above objectives, the present invention is implemented by the following technical scheme: a method for separating pesticide active substances from waste lavender straw, specifically comprising the following separation steps: Step 1: Pretreatment: Wash 120g-170g of lavender waste straw, and then crush, grind and sieve it in sequence; Step 2, extraction: adding a solvent to the treated waste lavender straw, and subjecting it to ultrasonic treatment using an ultrasonic instrument; Step 3, primary filtration: Pour in 1200mL-1500mL of ethanol solution, heat under reflux for 50min-65min, and filter to obtain filtrate 1; Step 4, secondary filtration: Pour 850mL-1000mL of ethanol solution into the filtered residue, continue to extract once, and then filter to obtain filtrate 2, and mix filtrate 2 with filtrate 1 in step 3 to obtain a mixed filtrate containing pesticide active substances; Step 5, primary purification: add solvent to the mixed filtrate of step 4, pour into a separatory funnel, first fully shake for 3min-5min, then stand for 10min-30min to allow the solution to separate into layers, and collect the supernatant; Step 6. Secondary purification: Load the supernatant onto the SPE column at a flow rate of 1 mL / min-2 mL / min. During this process, the active substances of the pesticide are adsorbed on the column filler, and some impurities flow out with the solvent. Then, the SPE column is rinsed with a washing solvent.

[0005] Preferably, in the step 1, the product is sieved through a 60-80 mesh sieve.

[0006] Preferably, in step 2, the solvent is methanol.

[0007] Preferably, in the step 2, the mass ratio of the solvent to the solid is 1:(5-15), the ultrasonic treatment time is 30 min-60 min, and the ultrasonic treatment temperature is 30°C-70°C.

[0008] Preferably, in step three and step four, the mass fraction of the ethanol solution used is 65%-75%; and a 0.5 μm ceramic membrane is used for filtration.

[0009] Preferably, in step six, if the pesticide active substance in the waste lavender straw is acidic, a silica gel bonded C18 column is used, and the washing solvent is selected from any one of a methanol aqueous solution or an acetonitrile aqueous solution.

[0010] Preferably, in step six, if the pesticide active substance in the waste lavender straw is alkaline, an amino column is used, and the washing solvent is selected from any one of deionized water, methanol, and n-hexane.

[0011] Preferably, in step six, the sample volume is 60 mL-68 mL, and the volume of the washing solvent is 3 mL-8 mL.

[0012] A method for separating pesticide active substances from waste lavender straws and its application in separating pesticide active substances. Beneficial Effects

[0013] The present invention provides a method for separating pesticide active substances from waste lavender straw and its application. Compared with the prior art, it has the following beneficial effects: (1) The separation method and application of pesticide active substances from waste lavender straw adopts an ethanol solution for two filtrations, so that the first filtration can remove some larger impurity particles, and the second filtration is based on the preliminary purification, further removing the tiny impurities that may remain in the ethanol solution, which can effectively purify the sample, thereby improving the purity of the pesticide active substances; and the two filtrations are helpful to accurately separate the target pesticide active substances; ethanol as a solvent can dissolve the pesticide active substances, and filtration can exclude other interfering components, so that the subsequent extraction of the pesticide active substances or further separation operations are more effective, thereby improving the accuracy of separation.

[0014] (2) The separation method and application of the pesticide active substances from the waste lavender straw can effectively remove a large amount of water-soluble impurities through two purification treatments, and at the same time, the pesticide active substances can be enriched in the organic phase or the target phase, thereby increasing the relative content of the target substance, which is beneficial to subsequent treatment; at the same time, the residual impurities, such as trace amounts of pigments, organic acids, etc., can be further removed through the SPE column to obtain purer pesticide active substances; at the same time, the SPE column can also play a concentrating role. During the elution process, a smaller volume of elution solvent can be used to elute the pesticide active substances adsorbed on the column, thereby increasing the concentration of the pesticide active substances, which is beneficial to subsequent analysis and detection and improves the sensitivity of detection. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 A comparison chart of average yields of pesticide active substances provided for a method for separating pesticide active substances from waste lavender straw and application of the present invention. DETAILED DESCRIPTION

[0016] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0017] In the technical scheme, the pesticide active substances of the waste lavender straw in Examples 1 and 2 are acidic, and the pesticide active substances of the waste lavender straw in Examples 3 and 4 are alkaline. Example

[0018] A method for separating pesticide active substances from waste lavender straw, specifically comprising the following separation steps: Step 1: Pretreatment: Wash 120 g of lavender waste straw, and then crush, grind and pass through a 60-mesh sieve in sequence; Step 2, extraction: adding methanol to the treated lavender waste straw, with a mass ratio of methanol to solid being 1:5, and subjecting it to ultrasonic treatment using an ultrasonic instrument, wherein the ultrasonic treatment time is 30 minutes and the ultrasonic treatment temperature is 30° C.; Step 3, primary filtration: Pour in 1200 mL of 65% ethanol solution, heat and reflux for extraction for 50 min, and filter using a 0.5 μm ceramic membrane to obtain filtrate 1; Step 4, secondary filtration: Pour 850 mL of 65% ethanol solution into the filtered residue, continue extraction once, and then filter with a 0.5 μm ceramic membrane to obtain filtrate 2, and mix filtrate 2 with filtrate 1 in step 3 to obtain a mixed filtrate containing pesticide active substances; Step 5, primary purification: add solvent to the mixed filtrate of step 4, pour into a separatory funnel, fully shake for 3 minutes, then stand for 10 minutes to allow the solution to separate, and collect the supernatant; Step 6, secondary purification: The supernatant was loaded onto a silica-bonded C18 column at a flow rate of 1 mL / min, with a loading volume of 60 mL. During this process, the pesticide active substances were adsorbed on the column filler, and some impurities flowed out with the solvent. The SPE column was then rinsed with a 3 mL methanol-water solution. Example

[0019] A method for separating pesticide active substances from waste lavender straw, specifically comprising the following separation steps: Step 1: Pretreatment: Wash 150 g of lavender waste straw, and then crush, grind and pass through a 70-mesh sieve in sequence; Step 2, extraction: adding methanol to the treated lavender waste straw, with a mass ratio of methanol to solid being 1:10, and subjecting it to ultrasonic treatment using an ultrasonic instrument, wherein the ultrasonic treatment time is 45 minutes and the ultrasonic treatment temperature is 50° C.; Step 3, primary filtration: Pour in 1300 mL of 70% ethanol solution, heat under reflux for 55 min, and filter with a 0.5 μm ceramic membrane to obtain filtrate 1; Step 4, secondary filtration: Pour 900 mL of 70% ethanol solution into the filtered residue, continue extraction once, and then filter with a 0.5 μm ceramic membrane to obtain filtrate 2, and mix filtrate 2 with filtrate 1 in step 3 to obtain a mixed filtrate containing pesticide active substances; Step 5, primary purification: add solvent to the mixed filtrate of step 4, pour into a separatory funnel, fully shake for 4 minutes, then stand for 20 minutes to allow the solution to separate, and collect the supernatant; Step 6, secondary purification: The supernatant was loaded onto a silica-bonded C18 column at a flow rate of 1.5 mL / min, with a loading volume of 64 mL. During this process, the pesticide active substances were adsorbed on the column filler, and some impurities flowed out with the solvent. The SPE column was then rinsed with 5 mL of acetonitrile aqueous solution. Example

[0020] A method for separating pesticide active substances from waste lavender straw, specifically comprising the following separation steps: Step 1: Pretreatment: Wash 160 g of lavender waste straw, and then crush, grind and pass through a 75-mesh sieve in sequence; Step 2, extraction: adding methanol to the treated lavender waste straw, with a mass ratio of methanol to solid being 1:14, and subjecting it to ultrasonic treatment using an ultrasonic instrument, wherein the ultrasonic treatment time is 50 minutes and the ultrasonic treatment temperature is 60°C; Step 3, primary filtration: Pour in 1400 mL of 72% ethanol solution, heat under reflux for 60 min, and filter using a 0.5 μm ceramic membrane to obtain filtrate 1; Step 4, secondary filtration: Pour 950 mL of 70% ethanol solution into the filtered residue, continue extraction once, and then filter with a 0.5 μm ceramic membrane to obtain filtrate 2, and mix filtrate 2 with filtrate 1 in step 3 to obtain a mixed filtrate containing pesticide active substances; Step 5, primary purification: add solvent to the mixed filtrate of step 4, pour into a separatory funnel, fully shake for 3 minutes, then stand for 25 minutes to allow the solution to separate, and collect the supernatant; Step 6, secondary purification: The supernatant was loaded onto the amino column at a flow rate of 2 mL / min, and the loading volume was 66 mL. During this process, the pesticide active substances were adsorbed on the column filler, and some impurities flowed out with the solvent. Then, the SPE column was rinsed with 6 mL of deionized water. Example

[0021] A method for separating pesticide active substances from waste lavender straw, specifically comprising the following separation steps: Step 1: Pretreatment: Wash 170 g of lavender waste straw, and then crush, grind and pass through an 80-mesh sieve in sequence; Step 2, extraction: adding methanol to the treated lavender waste straw, with a mass ratio of methanol to solid being 1:15, and subjecting it to ultrasonic treatment using an ultrasonic instrument, wherein the ultrasonic treatment time is 60 minutes and the ultrasonic treatment temperature is 70°C; Step 3, primary filtration: Pour in 1500 mL of 75% ethanol solution, heat under reflux for 65 min, and filter using a 0.5 μm ceramic membrane to obtain filtrate 1; Step 4, secondary filtration: Pour 1000 mL of 75% ethanol solution into the filtered residue, continue extraction once, and then filter with a 0.5 μm ceramic membrane to obtain filtrate 2, and mix filtrate 2 with filtrate 1 in step 3 to obtain a mixed filtrate containing pesticide active substances; Step 5, primary purification: add solvent to the mixed filtrate of step 4, pour into a separatory funnel, fully shake for 5 minutes, then stand for 30 minutes to allow the solution to separate, and collect the supernatant; Step 6, secondary purification: The supernatant was loaded onto the amino column at a flow rate of 2 mL / min, and the loading volume was 68 mL. During this process, the pesticide active substances were adsorbed on the column filler, and some impurities flowed out with the solvent. Then, the SPE column was rinsed with 8 mL of n-hexane.

[0022] Comparative Example 1 A method for separating pesticide active substances from waste lavender straw, specifically comprising the following separation steps: Step 1: Pretreatment: Wash 120 g of lavender waste straw, and then crush, grind and pass through a 60-mesh sieve in sequence; Step 2, extraction: adding methanol to the treated lavender waste straw, with a mass ratio of methanol to solid being 1:5, and subjecting it to ultrasonic treatment using an ultrasonic instrument, wherein the ultrasonic treatment time is 30 minutes and the ultrasonic treatment temperature is 30° C.; Step 3, filtration: Pour in 1200 mL of 65% ethanol solution, heat and reflux for 50 minutes, and filter with a 0.5 μm ceramic membrane to obtain a mixed filtrate containing pesticide active substances; Step 4: Primary purification: Add solvent to the filtrate, pour into a separatory funnel, shake thoroughly for 3 minutes, then let stand for 10 minutes to allow the solution to separate into layers, and collect the supernatant; Step 5, secondary purification: The supernatant was loaded onto a silica-bonded C18 column at a flow rate of 1 mL / min, with a loading volume of 60 mL. During this process, the active substances of the pesticide were adsorbed on the column filler, and some impurities flowed out with the solvent. Then, the SPE column was rinsed with a methanol-water solution with a volume of 3 mL.

[0023] Comparative Example 2 A method for separating pesticide active substances from waste lavender straw, specifically comprising the following separation steps: Step 1: Pretreatment: Wash 120 g of lavender waste straw, and then crush, grind and pass through a 60-mesh sieve in sequence; Step 2, extraction: adding methanol to the treated lavender waste straw, with a mass ratio of methanol to solid being 1:5, and subjecting it to ultrasonic treatment using an ultrasonic instrument, wherein the ultrasonic treatment time is 30 minutes and the ultrasonic treatment temperature is 30° C.; Step 3, filtration: Pour in 1200 mL of 65% ethanol solution, heat and reflux for 50 minutes, and filter with a 0.5 μm ceramic membrane to obtain a mixed filtrate containing pesticide active substances; Step 4: Purification: Add solvent to the mixed filtrate, pour into a separatory funnel, shake thoroughly for 3 minutes, then let stand for 10 minutes to allow the solution to separate, and collect the supernatant.

[0024] Comparative Example 3 A method for separating pesticide active substances from waste lavender straw, specifically comprising the following separation steps: Step 1: Pretreatment: Wash 160 g of lavender waste straw, and then crush, grind and pass through a 70-mesh sieve in sequence; Step 2, extraction: adding methanol to the treated lavender waste straw, with a mass ratio of methanol to solid being 1:14, and subjecting it to ultrasonic treatment using an ultrasonic instrument, wherein the ultrasonic treatment time is 50 minutes and the ultrasonic treatment temperature is 60°C; Step 3, filtration: Pour in 1400 mL of 72% ethanol solution, heat under reflux for 60 min, and filter using a 0.5 μm ceramic membrane to obtain a mixed filtrate containing pesticide active substances; Step 4: Purification: Load the mixed filtrate onto the amino column at a flow rate of 2 mL / min with a loading volume of 66 mL. During this process, the pesticide active substances are adsorbed on the column filler and some impurities flow out with the solvent. Then, the SPE column is rinsed with 6 mL of deionized water.

[0025] Determination of pesticide active substance content: Determination conditions: 1.0 cm cuvette; wavelength 560 nm; calculate the average yield of pesticide active substances based on the content; the results are as follows Figure 1 As shown: compared with Comparative Examples 1-3, the average yield of pesticide active substances in Examples 1-4 is significantly improved.

[0026] Meanwhile, the contents not described in detail in this specification belong to the prior art known to those skilled in the art.

[0027] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.

[0028] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for separating pesticide active substances from waste lavender straw, characterized in that: The specific separation steps include: Step 1: Pretreatment: Wash 120g-170g of lavender waste straw, and then crush, grind and sieve it in sequence; Step 2, extraction: adding a solvent to the treated waste lavender straw, and subjecting it to ultrasonic treatment using an ultrasonic instrument; Step 3, primary filtration: Pour in 1200mL-1500mL of ethanol solution, heat under reflux for 50min-65min, and filter to obtain filtrate 1; Step 4, secondary filtration: Pour 850mL-1000mL of ethanol solution into the filtered residue, continue to extract once, and then filter to obtain filtrate 2, and mix filtrate 2 with filtrate 1 in step 3 to obtain a mixed filtrate containing pesticide active substances; Step 5, primary purification: add solvent to the mixed filtrate of step 4, pour into a separatory funnel, first fully shake for 3min-5min, then stand for 10min-30min to allow the solution to separate into layers, and collect the supernatant; Step 6. Secondary purification: Load the supernatant onto the SPE column at a flow rate of 1 mL / min-2 mL / min. During this process, the active substances of the pesticide are adsorbed on the column filler, and some impurities flow out with the solvent. Then, the SPE column is rinsed with a washing solvent.

2. A method for separating pesticide active substances from waste lavender straw according to claim 1, characterized in that: In the step 1, the product is sieved through a 60-80 mesh sieve.

3. A method for separating pesticide active substances from waste lavender straw according to claim 1, characterized in that: In the step 2, the solvent is methanol.

4. The method for separating pesticide active substances from waste lavender straw according to claim 1, characterized in that: In the step 2, the mass ratio of the solvent to the solid is 1:(5-15), the ultrasonic treatment time is 30 min-60 min, and the ultrasonic treatment temperature is 30° C.-70° C.

5. The method for separating pesticide active substances from waste lavender straw according to claim 1, characterized in that: In the step 3 and the step 4, the mass fraction of the ethanol solution used is 65%-75%; and a 0.5 μm ceramic membrane is used for filtration.

6. The method for separating pesticide active substances from waste lavender straw according to claim 1, characterized in that: In step six, if the pesticide active substance in the waste lavender straw is acidic, a silica gel bonded C18 column is used, and the washing solvent is selected from any one of a methanol aqueous solution or an acetonitrile aqueous solution.

7. The method for separating pesticide active substances from waste lavender straw according to claim 1, characterized in that: In step six, if the pesticide active substances in the waste lavender straw are alkaline, an amino column is used, and the washing solvent is selected from any one of deionized water, methanol, and n-hexane.

8. The method for separating pesticide active substances from waste lavender straw according to claim 1, characterized in that: In the step six, the sample volume is 60 mL-68 mL, and the volume of the washing solvent is 3 mL-8 mL.

9. Use of the method for separating pesticide active substances from waste lavender straw according to claim 1 in separating pesticide active substances.

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