Composition for removing pesticide residues, preparation method of composition and application of composition in preparation of pure white capsules

Abstract

The invention belongs to the field of washing products, and particularly relates to a composition for removing pesticide residues, a preparation method of the composition and application of the composition in preparation of pure white capsules. The composition is prepared from the following raw materials: shell powder, table salt, citric acid, sodium carbonate, sodium percarbonate, flos chrysanthemi, radix arnebiae seu lithospermi, flos lonicerae, fructus gleditsiae, bamboo leaves, tea seeds, radix bupleuri, herba menthae, cocamidopropyl betaine, sucrose ester and lauryl sodium sulfate. The cleaning composition for removing pesticide residues in traditional Chinese medicines is obtained by selecting specific raw materials and proportions, and the composition greatly improves the pesticide removal rate of the raw materials in the pure white capsule.

Description

Technical Field

[0001] The invention belongs to the field of washing products, and in particular relates to a composition for removing pesticide residues, a preparation method thereof and application of the composition in preparing whitening capsules. Background Art

[0002] In a broad sense, pesticides refer to chemical drugs used to control harmful organisms that endanger agricultural, forestry and animal husbandry production and regulate plant growth. They mainly include organophosphorus, carbamate, organic nitrogen, pyrethroid and organochlorine pesticides.

[0003] Chinese herbal medicines are agricultural and sideline products. Therefore, in the process of planting, growers usually use a large amount of pesticides to ensure production and prevent pests and diseases. Pesticide residues will cause pollution to Chinese herbal medicines. After people take Chinese medicines with excessive pesticide residues, the toxic and harmful components of the pesticides will accumulate in the body, which will cause harm to people who are directly or indirectly treating diseases. With the continuous expansion of the scope and amount of pesticide use, it is necessary to control pesticide residues. In the process of removing pesticide residues from Chinese herbal medicines, the general Chinese herbal medicine removal device uses a cleaning liquid and Chinese herbal medicines to mix and then stir.

[0004] Jiebai Capsule is a Chinese patent medicine. Its main ingredients include Terminalia chebula, nutmeg, cloves, agarwood, etc. It has the effects of strengthening the spleen and stomach, relieving pain and vomiting, and separating clear and turbid substances. It is used to treat symptoms such as abdominal distension and pain, indigestion, and difficulty urinating. Before preparing the medicine, the Chinese medicinal materials need to be cleaned to remove pesticide residues.

[0005] Chinese invention patent application CN101732819A discloses an organophosphorus degrading enzyme preparation and a preparation method thereof. The method uses an organophosphorus pesticide degrading enzyme to degrade pesticides remaining on vegetables and fruits. However, the biological enzyme used in the method is relatively expensive, and the activity of the enzyme is easily affected by the surrounding environment.

[0006] Chinese invention patent application CN102499335A discloses a method for rapidly degrading organophosphorus pesticides in fruits and vegetables using a nano-degradation agent. The method uses a nano-degradation agent whose active ingredient is nano-TiO2 to rapidly degrade organophosphorus pesticides in fruits and vegetables under natural light. However, nano-TiO2 is toxic to the human body.

[0007] Chinese invention patent application CN106689978A discloses a method for removing organophosphorus pesticides from the surface of vegetables. The method combines ultraviolet irradiation and dynamic cleaning with ozone water to degrade the pesticides in the vegetables. However, the method has complex steps, is time-consuming, and requires the addition of potassium permanganate chemical reagents to the clean water.

[0008] Therefore, it is necessary to develop a cleaning agent that is easy to use, non-toxic / non-polluting, and has excellent cleaning effect to remove pesticide residues on the surface of medicinal materials used in the preparation of white capsules. Summary of the invention

[0009] In view of the deficiencies in the prior art, the present invention provides a composition for removing pesticide residues, a preparation method thereof, and an application of the composition in preparing white capsules.

[0010] In order to achieve the above-mentioned purpose of the present invention, the specific technical solution adopted by the present invention is:

[0011] A composition for removing pesticide residues. The raw materials of the composition include shell powder, salt, citric acid, sodium carbonate, sodium percarbonate, chrysanthemum, lithospermum officinale, honeysuckle, sapodilla, bamboo leaves, tea seeds, bupleurum, mint, cocoamidopropyl betaine, sucrose ester and sodium lauryl sulfate.

[0012] Preferably, the raw materials of the composition include, by weight: 30-40 parts of shell powder, 5-10 parts of salt, 2-5 parts of citric acid, 4-6 parts of sodium carbonate, 4-6 parts of sodium percarbonate, 12-18 parts of chrysanthemum, 10-15 parts of lithospermum, 10-15 parts of honeysuckle, 15-20 parts of sapodilla, 8-12 parts of bamboo leaves, 20-25 parts of tea seeds, 10-15 parts of bupleurum, 8-12 parts of mint, 10-12 parts of cocoyl betaine, 8-12 parts of sucrose ester and 10-15 parts of sodium lauryl sulfate.

[0013] Further preferably, the raw materials of the composition include, by weight: 35 parts of shell powder, 8 parts of salt, 4 parts of citric acid, 5 parts of sodium carbonate, 5 parts of sodium percarbonate, 14 parts of chrysanthemum, 12 parts of comfrey, 13 parts of honeysuckle, 17 parts of sapodilla, 10 parts of bamboo leaves, 24 parts of tea seeds, 12 parts of bupleurum, 10 parts of mint, 11 parts of cocoyl betaine, 10 parts of sucrose ester and 14 parts of sodium lauryl sulfate.

[0014] Preferably, the method for preparing the shell powder comprises the following steps:

[0015] After the shells are cleaned, they are soaked in hydrochloric acid and then in sodium hydroxide, dried, crushed, calcined, cooled, and crushed to obtain shell powder.

[0016] Further preferably, the time for the hydrochloric acid impregnation and the sodium hydroxide impregnation is 30-50 minutes; the calcination procedure is: calcination at 400°C for 30-60 minutes, heating to 800°C for 30-60 minutes, and then heating to 1200°C for 30-60 minutes.

[0017] Furthermore, the shells are derived from one or more of mussel shells, scallop shells, oyster shells, flower shells and river clam shells.

[0018] The present invention also relates to a method for preparing the above composition, comprising the following steps:

[0019] (1) Gleditsia sinensis, tea seeds and mint are crushed and mixed, subjected to ultrasonic extraction with solvent A, concentrated and dried to obtain extract 1;

[0020] (2) crushing chrysanthemum, lithospermum officinale, honeysuckle, bamboo leaves and radix bupleuri, mixing, adding water, heating for extraction, concentrating and drying to obtain extract 2;

[0021] (3) Extract 1, extract 2, shell powder, salt, citric acid, sodium carbonate, sodium percarbonate, cocoyl propyl betaine, sucrose ester and sodium lauryl sulfate are mixed to obtain the composition.

[0022] Preferably, the solvent A in step (1) is a mixed solution of betaine, citric acid, ethanol and water, and the mass ratio of betaine, citric acid, ethanol and water is 0.5-1:1-2:40-50:10-20.

[0023] Preferably, the amount of solvent A added in step (1) is 8-10 times the total mass of sapodilla, tea seed and mint, the temperature of ultrasonic extraction is 50-70°C, the time of ultrasonic extraction is 50-70min, and the power of ultrasound is 200-400W.

[0024] Preferably, the temperature of the heating extraction in step (2) is 80-90° C., the number of heating extractions is 2-3 times, each extraction lasts 1-2 hours, the amount of water added during each extraction is 8-10 times the total mass of chrysanthemum, lithospermum, honeysuckle, bamboo leaves and bupleurum, and the extracts are combined after heating extraction.

[0025] The present invention also relates to the use of the above composition or the composition prepared by the above preparation method in preparing a cleaning agent for removing pesticide residues.

[0026] The present invention also relates to the application of the composition or the composition prepared by the preparation method in the preparation of white capsules.

[0027] Compared with the prior art, the present invention has the following beneficial effects:

[0028] (1) The present invention obtains a cleaning composition for removing pesticide residues in traditional Chinese medicine by selecting specific raw materials and proportions. The composition greatly improves the pesticide removal rate of the raw materials used in the whitening capsule and significantly reduces the pesticide residues in the traditional Chinese medicine. At the same time, there is a significant synergistic effect between the surfactant cocoyl propyl betaine and sucrose ester.

[0029] (2) The present invention obtains a composition with better cleaning effect through a specific preparation method. The preparation method can significantly reduce the pesticide residues in the raw materials of the white capsules, has obvious technical advantages over conventional preparation processes, and the preparation method is simple, low-cost, and suitable for industrial production. DETAILED DESCRIPTION

[0030] The present invention will be further described in detail below in conjunction with specific examples. The following examples are not intended to limit the present invention, but are only intended to illustrate the present invention. The experimental methods used in the following examples are generally conventional, unless otherwise specified, and the materials, reagents, etc. used in the following examples are commercially available, unless otherwise specified.

[0031] Example 1

[0032] A composition for removing pesticide residues, comprising the following raw materials by weight: 35 parts of shell powder, 8 parts of salt, 4 parts of citric acid, 5 parts of sodium carbonate, 5 parts of sodium percarbonate, 14 parts of chrysanthemum, 12 parts of lithospermum, 13 parts of honeysuckle, 17 parts of sapodilla, 10 parts of bamboo leaves, 24 parts of tea seeds, 12 parts of bupleurum, 10 parts of mint, 11 parts of cocoyl propyl betaine, 10 parts of sucrose ester and 14 parts of sodium lauryl sulfate.

[0033] The preparation method of shell powder is as follows: after cleaning the mussel shells, soak them in hydrochloric acid for 40 minutes, then soak them in sodium hydroxide for 40 minutes, dry and crush them, calcine them at 400°C for 40 minutes, heat them to 800°C for 50 minutes, then heat them to 1200°C for 40 minutes, cool them, crush them, and obtain shell powder.

[0034] The preparation method of the above composition is:

[0035] (1) Gleditsia sinensis, tea seeds and mint were crushed and mixed, and 9 times the mass of solvent A (a mixed solution of betaine, citric acid, ethanol and water in a mass ratio of 0.7:1.5:45:15) was added, and ultrasonic extraction was performed at 60° C. for 60 min with an ultrasonic power of 300 W. The extract was concentrated and dried to obtain extract 1;

[0036] (2) crushing chrysanthemum, lithospermum, honeysuckle, bamboo leaves and bupleurum, mixing, adding water, heating and extracting at 85° C. for 1.5 h, heating and extracting twice, wherein the amount of water added each time is 9 times the total weight of chrysanthemum, lithospermum, honeysuckle, bamboo leaves and bupleurum, combining the extracts after heating and extracting, concentrating and drying, and obtaining extract 2;

[0037] (3) Extract 1, extract 2, shell powder, salt, citric acid, sodium carbonate, sodium percarbonate, cocoyl propyl betaine, sucrose ester and sodium lauryl sulfate are mixed to obtain the composition.

[0038] Example 2

[0039] A composition for removing pesticide residues, comprising the following raw materials by weight: 30 parts of shell powder, 5 parts of salt, 2 parts of citric acid, 4 parts of sodium carbonate, 4 parts of sodium percarbonate, 12 parts of chrysanthemum, 10 parts of lithospermum, 10 parts of honeysuckle, 15 parts of sapodilla, 8 parts of bamboo leaves, 20 parts of tea seeds, 10 parts of bupleurum, 8 parts of mint, 10 parts of cocoamidopropyl betaine, 8 parts of sucrose ester and 10 parts of sodium lauryl sulfate.

[0040] The preparation method of shell powder is as follows: after cleaning the mussel shells, soak them in hydrochloric acid for 30 minutes, then soak them in sodium hydroxide for 30 minutes, dry and crush them, calcine them at 400°C for 30 minutes, heat them to 800°C for 60 minutes, then heat them to 1200°C for 60 minutes, cool them, crush them, and obtain shell powder.

[0041] The preparation method of the above composition is:

[0042] (1) Gleditsia sinensis, tea seeds and mint were crushed and mixed, and 8 times the mass of solvent A (a mixed solution of betaine, citric acid, ethanol and water in a mass ratio of 0.5:1:40:10) was added, and ultrasonic extraction was performed at 50° C. for 70 min with an ultrasonic power of 200 W, and the extract was concentrated and dried to obtain extract 1;

[0043] (2) crushing chrysanthemum, lithospermum, honeysuckle, bamboo leaves and bupleurum, mixing, adding water, heating and extracting at 80° C. for 2 h, heating and extracting for 3 times, wherein the amount of water added in each extraction is 8 times the total weight of chrysanthemum, lithospermum, honeysuckle, bamboo leaves and bupleurum, combining the extracts after heating and extracting, concentrating and drying to obtain extract 2;

[0044] (3) Extract 1, extract 2, shell powder, salt, citric acid, sodium carbonate, sodium percarbonate, cocoyl propyl betaine, sucrose ester and sodium lauryl sulfate are mixed to obtain the composition.

[0045] Example 3

[0046] A composition for removing pesticide residues comprises the following raw materials by weight: 40 parts of shell powder, 10 parts of salt, 5 parts of citric acid, 6 parts of sodium carbonate, 6 parts of sodium percarbonate, 18 parts of chrysanthemum, 15 parts of lithospermum, 15 parts of honeysuckle, 20 parts of sapodilla, 12 parts of bamboo leaves, 25 parts of tea seeds, 15 parts of bupleurum, 12 parts of mint, 12 parts of cocoamidopropyl betaine, 12 parts of sucrose ester and 15 parts of sodium lauryl sulfate.

[0047] The preparation method of shell powder is as follows: after cleaning the mussel shells, soak them in hydrochloric acid for 50 minutes, then soak them in sodium hydroxide for 50 minutes, dry and crush them, calcine them at 400°C for 60 minutes, heat them to 800°C for 30 minutes, then heat them to 1200°C for 30 minutes, cool them, crush them, and obtain shell powder.

[0048] The preparation method of the above composition is:

[0049] (1) Gleditsia sinensis, tea seeds and mint were crushed and mixed, and 10 times the mass of solvent A (a mixed solution of betaine, citric acid, ethanol and water in a mass ratio of 1:2:50:20) was added, and ultrasonic extraction was performed at 70° C. for 50 min with an ultrasonic power of 400 W, and the extract was concentrated and dried to obtain extract 1;

[0050] (2) crushing chrysanthemum, lithospermum, honeysuckle, bamboo leaves and bupleurum, mixing, adding water, heating and extracting at 90° C. for 1 h, heating and extracting twice, wherein the amount of water added each time is 10 times the total weight of chrysanthemum, lithospermum, honeysuckle, bamboo leaves and bupleurum, combining the extracts after heating and extracting, concentrating and drying to obtain extract 2;

[0051] (3) Extract 1, extract 2, shell powder, salt, citric acid, sodium carbonate, sodium percarbonate, cocoyl propyl betaine, sucrose ester and sodium lauryl sulfate are mixed to obtain the composition.

[0052] Comparative Example 1

[0053] The difference between this comparative example and Example 1 is that the raw material ratio is different, which is as follows:

[0054] The raw materials of the composition are, by weight, 10 parts of shell powder, 20 parts of salt, 4 parts of citric acid, 3 parts of sodium carbonate, 7 parts of sodium percarbonate, 20 parts of chrysanthemum, 8 parts of lithospermum, 13 parts of honeysuckle, 25 parts of sapodilla, 10 parts of bamboo leaves, 24 parts of tea seeds, 12 parts of bupleurum, 13 parts of mint, 5 parts of cocoyl propyl betaine, 22 parts of sucrose ester and 8 parts of sodium lauryl sulfate.

[0055] Comparative Example 2

[0056] The difference between this comparative example and Example 1 is that the added amounts of cocoamidopropyl betaine and sucrose ester are different, specifically: 21 parts of cocoamidopropyl betaine and 0 parts of sucrose ester.

[0057] Comparative Example 3

[0058] The difference between this comparative example and Example 1 is that the added amounts of cocoamidopropyl betaine and sucrose ester are different, specifically: 0 parts of cocoamidopropyl betaine and 21 parts of sucrose ester.

[0059] Comparative Example 4

[0060] The only difference between this comparative example and Example 1 is that honeysuckle and bamboo leaves are replaced by camellia and sedge respectively.

[0061] Comparative Example 5

[0062] The only difference between this comparative example and Example 1 is that the composition of solvent A in step (1) of the preparation method is: betaine, citric acid and water in a mass ratio of 0.7:1.5:15.

[0063] Comparative Example 6

[0064] The difference between this comparative example and Example 1 is that the preparation method is different, which is as follows:

[0065] (1) Gleditsia sinensis, tea seeds, mint, chrysanthemum, lithospermum officinale, honeysuckle, bamboo leaves and radix bupleuri are crushed, mixed, and water is added. The mixture is heated and extracted at 85° C. for 1.5 h. The heating extraction is repeated twice. The amount of water added each time is 9 times the total weight of the raw materials. After the heating extraction, the extracts are combined, concentrated and dried to obtain an extract.

[0066] (2) The extract, shell powder, salt, citric acid, sodium carbonate, sodium percarbonate, cocoyl propyl betaine, sucrose ester and sodium lauryl sulfate are mixed to obtain the composition.

[0067] Effect test

[0068] The compositions prepared in Examples 1-3 and Comparative Examples 1-6 were respectively mixed with water at a mass ratio of 1:1000 to obtain cleaning agents.

[0069] The detection is based on the pesticide residue determination method 2341 in the general chapter 4 of the 2020 edition of the Chinese Pharmacopoeia.

[0070] The above cleaning agent was used to test the removal of pesticide residues from the raw materials of the white capsules, namely, myristicin, nutmeg and tsaoko kernel. The specific method is as follows:

[0071] Take chebula, divide it into 11 equal parts, spray it with fenamiphos, place it at room temperature for 24 hours, dry it, take samples respectively, detect the fenamiphos pesticide content, then wash 10 parts of chebula with the composition of Examples 1-3 and Comparative Examples 1-6 respectively, and take out 1 part without treatment (blank control group). The washing method is: soak the chebula in a cleaning agent respectively, ultrasonically treat it at 35°C and 300W for 15 minutes, and then rinse it with running clean water for 30 seconds; detect the residual amount of fenamiphos after washing, and calculate the removal rate (%) of fenamiphos.

[0072] The removal rates of DDT, carbofuran and fipronil sprayed on Terminalia chebula were tested according to the above method. The test results are shown in Table 1.

[0073] In addition, the above raw material Terminalia chebula was replaced by nutmeg and Amomum villosum kernel respectively, and the detection methods were consistent. The detection results are shown in Tables 2 and 3.

[0074] Table 1 Pesticide removal rate on the surface of Terminalia chebula

[0075]

[0076] Table 2 Pesticide removal rate on nutmeg surface

[0077]

[0078]

[0079] Table 3 Pesticide removal rate on the surface of grass kernels

[0080]

[0081] It can be seen from Tables 1 to 3 that the cleaning effects of the compositions prepared in Examples 1-3 are better than those in Comparative Examples 1-6. The cleaning composition of the present invention significantly reduces the pesticide residues in the white capsules, and the preparation method is simple, low-cost, and suitable for industrial production.

[0082] The above detailed description is a specific description of one feasible embodiment of the present invention. The embodiment is not intended to limit the patent scope of the present invention. Any equivalent implementation or modification that does not deviate from the present invention should be included in the scope of the technical solution of the present invention.

Claims

1. A composition for removing pesticide residues, characterized in that: The raw materials of the composition include shell powder, salt, citric acid, sodium carbonate, sodium percarbonate, chrysanthemum, comfrey, honeysuckle, sapodilla, bamboo leaf, tea seed, bupleurum, mint, cocoyl propyl betaine, sucrose ester and sodium lauryl sulfate.

2. The composition according to claim 1, characterized in that The raw materials of the composition include, by weight: 30-40 parts of shell powder, 5-10 parts of salt, 2-5 parts of citric acid, 4-6 parts of sodium carbonate, 4-6 parts of sodium percarbonate, 12-18 parts of chrysanthemum, 10-15 parts of lithospermum, 10-15 parts of honeysuckle, 15-20 parts of sapodilla, 8-12 parts of bamboo leaves, 20-25 parts of tea seeds, 10-15 parts of bupleurum, 8-12 parts of mint, 10-12 parts of cocoyl propyl betaine, 8-12 parts of sucrose ester and 10-15 parts of sodium lauryl sulfate.

3. The composition according to any one of claims 1 to 2, characterized in that The preparation method of the shell powder comprises the following steps: After the shells are cleaned, they are soaked in hydrochloric acid and then in sodium hydroxide, dried, crushed, calcined, cooled, and crushed to obtain shell powder.

4. The composition according to claim 3, characterized in that The time of the hydrochloric acid impregnation and the sodium hydroxide impregnation is 30-50 minutes; the calcination procedure is: calcination at 400°C for 30-60 minutes, heating to 800°C for 30-60 minutes, and then heating to 1200°C for 30-60 minutes.

5. A method for preparing the composition according to any one of claims 1 to 4, characterized in that: The following steps are involved: (1) Gleditsia sinensis, tea seeds and mint are crushed and mixed, subjected to ultrasonic extraction with solvent A, concentrated and dried to obtain extract 1; (2) crushing chrysanthemum, lithospermum officinale, honeysuckle, bamboo leaves and radix bupleuri, mixing, adding water, heating for extraction, concentrating and drying to obtain extract 2; (3) Extract 1, extract 2, shell powder, salt, citric acid, sodium carbonate, sodium percarbonate, cocoyl propyl betaine, sucrose ester and sodium lauryl sulfate are mixed to obtain the composition.

6. The preparation method according to claim 5, characterized in that: The solvent A in step (1) is a mixed solution of betaine, citric acid, ethanol and water, and the mass ratio of the betaine, citric acid, ethanol and water is 0.5-1:1-2:40-50:10-20.

7. The preparation method according to claim 5, characterized in that: The amount of solvent A added in step (1) is 8-10 times the total mass of sapodilla, tea seed and mint, the temperature of ultrasonic extraction is 50-70°C, the time of ultrasonic extraction is 50-70min, and the power of ultrasound is 200-400W.

8. The preparation method according to claim 5, characterized in that: The temperature of the heating extraction in step (2) is 80-90° C., the number of heating extractions is 2-3 times, each extraction lasts 1-2 hours, the amount of water added during each extraction is 8-10 times the total mass of chrysanthemum, lithospermum, honeysuckle, bamboo leaves and bupleurum, and the extracts are combined after heating extraction.

9. Use of the composition according to any one of claims 1 to 4 or the composition prepared by the preparation method according to any one of claims 5 to 8 in preparing a cleaning agent for removing pesticide residues.

10. Use of the composition according to any one of claims 1 to 4 or the composition prepared by the preparation method according to any one of claims 5 to 8 in preparing white capsules.

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