Fruit essence extraction method

Abstract

The invention discloses a fruit essence extraction method. The method comprises the following steps: extracting a fruit sample; grinding the sample; adding an organic solvent; extracting with an organic solvent; the method provided by the invention has the advantages of simple operation steps, short period, low energy consumption, wide applicability, full extraction and the like.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of pesticide residues, and particularly relates to a fruit essence extraction method and method. BACKGROUND

[0002] The history of spices is long, and people have collected tree bark and grass roots as medical products to drive away epidemics and impurities since the era of Huangdi and Shennong, which has a history of more than 5,000 years. At the beginning, people used these fragrant substances for worship, purification of the body and mind, and for sacrifice and funeral. Later, they were gradually used for food, decoration and beauty. In the 8th-10th century, people already knew how to separate spices by distillation. In 1370, the first kind of perfume extracted by ethanol, Eau de la Reimed Hongarie, appeared. It was initially distilled from rosemary, and then gradually from lavender and other plants. Since 1420, after the adoption of a serpentine condenser in distillation, essential oils have developed rapidly. Grasse, France, has become a world-renowned production base for natural spices (especially fragrant flowers) due to the production of flower oil and perfume. Since then, distillation has been gradually adopted to extract essential oils from citrus trees, flowers, fruits and leaves. This is a revolutionary progress that changes the solid fruits into liquids and extracts essential oils from fruits. Since the 18th century, due to the development of organic chemistry, people have made great progress in the extraction and component analysis of natural spices. With the continuous expansion of the application range of natural spices, the spice industry has developed rapidly, and the extraction technology of natural spices has been continuously improved.

[0003] Although the existing extraction method can achieve the preparation effect, it is easy to cause excessive consumption of fruit raw materials during the extraction process, increase the waste of raw materials and the cost of preparation, and cannot better guarantee the purity of plant essence after extraction, reduce the practicability and preparation quality, and cannot better store the extracted essence in the best state, which easily reduces the storage time of the essence and reduces the extraction effect. SUMMARY

[0004] The purpose of the present application is to provide a fruit essence extraction method, which has the advantages of simple operation steps, short cycle, low energy consumption, wide applicability, sufficient extraction, etc.

[0005] To achieve the above purpose, the present application provides the following technical scheme: a fruit essence extraction method, comprising the following steps: ①, extracting fruit samples; extracting 5-15 g of fruit at any position, adding deionized water for soaking, the volume of deionized water is 30-45 ml, the soaking time is 1-2 h, and ultrasonic instrument is used for ultrasonic treatment during the soaking process; ②, sample grinding; after soaking, the sample is ground by machine, squeezed, and the obtained liquid A and remaining residue B are collected and placed in a centrifuge tube and a beaker respectively; ③, adding organic solvent; adding organic solvent to liquid A, and adding the same organic solvent to the remaining residue B to obtain a solid-liquid mixture C; ④, organic solvent extraction; liquid A with organic solvent is allowed to stand for 1-2 hours, a dispersing agent is added to the obtained solid-liquid mixture C, after the addition of the dispersing agent is completed, stirring for 25-35 minutes, then an alkaline additive is added and heated and stirred for 60-85 minutes; ⑤, collecting filtrate: the liquid in the centrifuge tube is centrifuged to collect the supernatant D, the solid-liquid mixture in the beaker is naturally cooled to room temperature, and the supernatant is obtained by standing, the supernatant E is collected, and the supernatant D and the supernatant E are detected respectively, and the supernatant is collected to obtain the essence by standing.

[0006] As a preferred scheme of the present application, the organic solvent in step ③ uses benzene, acetone, diethyl ether, chloroform, etc.

[0007] As a preferred scheme of the present application, the volume ratio of the organic solvent to the deionized water is 1:1-1.5.

[0008] As a preferred scheme of the present application, the dispersing agent in step ④ uses any one of ethylene glycol and methanol.

[0009] As a preferred scheme of the present application, the volume ratio of the dispersing agent to the deionized water is 1:1-1.5.

[0010] As a preferred scheme of the present application, the alkaline additive in step ④ uses any one of polypyrrolidone, ethylenediamine and sodium acetate.

[0011] As a preferred scheme of the present application, the volume ratio of the liquid alkaline additive to the deionized water is 1:5-6, and the solid alkaline additive is 3-5 g.

[0012] As a preferred scheme of the present application, the temperature of heating and stirring in step ④ is 60-75℃, and the stirring speed is 25-35 r / min.

[0013] As a preferred scheme of the present application, the supernatant D and the supernatant E obtained in step 5 are detected respectively when the fruit is in a liquid state, and only the supernatant D is taken when the fruit is in a solid state.

[0014] It also includes distillation, including the following steps: ①, extract fruit sample; extract 5-15g at any position of the fruit, add deionized water for soaking, the volume of deionized water is 30-45ml, the soaking time is 1-2h, and ultrasonic instrument is used for ultrasonic in the soaking process; ②, sample crushing; the soaked sample is crushed by a mechanical crusher, and the obtained liquid A and the remaining residue B are collected and placed in a centrifugal tube and a beaker respectively; ③, adding organic solvent; the same organic solvent is added to the liquid A and the remaining residue B to obtain a solid-liquid mixture C; ④, organic solvent extraction; the liquid A added with the organic solvent is allowed to stand for 1-2h, a dispersing agent is added to the obtained solid-liquid mixture C, after the addition of the dispersing agent is completed, stirring is carried out for 25-35min, an alkaline additive is added after stirring, and heating and stirring are carried out for 60-85min; ⑤, collecting filtrate: the liquid in the centrifugal tube is subjected to centrifugal treatment, the upper clear liquid D is collected, the solid-liquid mixture in the beaker is naturally cooled to room temperature, the upper clear liquid E is collected by standing, and the upper clear liquids D and E are subjected to detection treatment respectively; ⑥, selecting the upper clear liquids D and E after detection, distilling the upper clear liquid with more organic matter content, and collecting the liquid after distillation to obtain essence.

[0015] Compared with the prior art, the present application has the advantages that: the present application uses an organic solvent that can fully dissolve organic phosphorus to extract organic phosphorus pesticide residues on the surface of fruits, and provides an effective extraction method for fruits in liquid and solid states. When the fruits are soaked, ultrasonic is used for full oscillation to reduce the firmness between fruit molecules, an organic solvent is added to the liquid to save the extraction step, and the extraction of organic phosphorus in fruits is carried out at low cost and high efficiency. For solid fruits, physical methods can be used to fully crush and release, and the water molecules residues in the fruits are fully extracted. At the same time, the remaining residues are fully dispersed and dissolved by using a dispersing agent, an organic solvent is added to the organic matter to fully dissolve the organic phosphorus, and the organic phosphorus residues in the fruits are maximized. Compared with the traditional sample pretreatment method, the present application has the advantages of simple operation steps, short cycle, low energy consumption, wide applicability, sufficient extraction, etc. BRIEF DESCRIPTION OF DRAWINGS

[0016] Figure 1 It is a step flowchart of the fruit essence extraction method of the present application; DETAILED DESCRIPTION

[0017] The technical solutions in the embodiments of the present application will be clearly and completely described with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative effort belong to the scope of the present application.

[0018] Please refer to Figure 1 The present application provides a technical solution: a fruit essence extraction method.

[0019] As Figure 1 shown, comprising the following steps: ①, extracting fruit samples; extracting 5-15g of any position of the fruit, adding deionized water for soaking, the volume of deionized water is 30-45ml, the soaking time is 1-2h, and ultrasonic instrument is used for ultrasonic treatment during the soaking process; ②, crushing the sample; the soaked sample is crushed by a mechanical crusher, and the obtained liquid A and the remaining residue B are collected and placed in a centrifugal tube and a beaker respectively; ③, adding organic solvent; adding organic solvent to liquid A and adding the same organic solvent to the remaining residue B to obtain a solid-liquid mixture C; ④, organic solvent extraction; liquid A with organic solvent is left to stand for 1-2h, dispersing agent is added to the obtained solid-liquid mixture C, after the addition of dispersing agent is completed, stirring for 25-35min, adding alkaline additive after stirring, heating and stirring for 60-85min, the temperature of heating and stirring is 60-75℃, and the stirring speed is 25-35r / min; ⑤, collecting filtrate: centrifugal treatment is performed on the liquid in the centrifugal tube, and the upper clear liquid D is collected, the solid-liquid mixture in the beaker is naturally cooled to room temperature, and the upper clear liquid E is collected after standing, and the upper clear liquid D and the upper clear liquid E are detected respectively.

[0020] In step ③, the organic solvent includes benzene, acetone, diethyl ether, chloroform and the like.

[0021] The volume ratio of the above-mentioned organic solvent to the deionized water is 1:1-1.5.

[0022] In step ④, the dispersing agent is any one of ethylene glycol and methanol.

[0023] The volume ratio of the above-mentioned dispersing agent to the deionized water is 1:1-1.5.

[0024] In step ④, the alkaline additive is any one of polypyrrolidone, ethylenediamine and sodium acetate.

[0025] and the volume ratio of the liquid basic additive to the deionized water is 1:5-6, wherein the solid basic additive is 3-5 g.

[0026] In step 5, the supernatant D obtained is used for detection when the fruit is in a liquid state, and the supernatant D and the supernatant E are detected respectively when the fruit is in a solid state.

[0027] The above scheme is used to perform the examples, and milk, fruits and vegetables, and meat are pretreated. The chemical reagents used in the above examples are commercially available chemical reagents, and the purity is analytical pure.

[0028] The organic solvent used is acetone, the dispersing agent is ethylene glycol, and the basic additive is ethylenediamine. Example

[0029] ①, extract the fruit sample; extract 10 g of milk to be detected, add deionized water for mixing, the volume of deionized water is 40 ml, the mixing time is 1.5 h, and ultrasonic instrument is used for ultrasonic during mixing; ②, add organic solvent; add 40 ml of acetone to the liquid after mixing is completed; ③, organic solvent extraction; the liquid to which acetone is added is allowed to stand for 1-2 h; ④, collect the filtrate: the liquid in the centrifugal tube is centrifuged to collect the supernatant, and the supernatant is detected; Example

[0030] ①, extract the fruit sample; extract 10 g of fruits and vegetables from any position, add deionized water for soaking, the volume of deionized water is 40 ml, the soaking time is 1-2 h, and ultrasonic instrument is used for ultrasonic during soaking; ②, crush the sample; the soaked sample is crushed by machine, and the obtained liquid A and the remaining residue B are collected and placed in centrifugal tubes and beakers respectively; ③, add organic solvent; add 40 ml of acetone to liquid A, and add the same amount of acetone to the remaining residue B to obtain a solid-liquid mixture C; ④, organic solvent extraction; the liquid A to which the organic solvent is added is allowed to stand for 1 h, a dispersing agent is added to the obtained solid-liquid mixture C, after 40 ml of ethylene glycol is added, stirring is performed for 25 min, 5 ml of ethylenediamine is added after stirring, heating and stirring are performed for 70 min, the temperature of heating and stirring is 70℃, and the stirring speed is 25 r / min; ⑤, collecting filtrate: centrifugal treatment is conducted on the liquid in the centrifugal tube, and the supernatant D is collected. The solid-liquid mixture in the beaker is naturally cooled to room temperature, and the supernatant is obtained by standing. The supernatant E is collected. The supernatant D and the supernatant E are respectively detected and treated, and the supernatant is collected. The essence is obtained by standing. Example

[0031] ①, extracting fruit samples; 10g of any position of meat food is added with deionized water for soaking. The volume of deionized water is 40ml, and the soaking time is 1h. Ultrasonic instrument is used for ultrasonic treatment during the soaking process; ②, sample crushing; the soaked sample is crushed and pressed by a machine. The obtained liquid A and the remaining residue B are respectively placed in a centrifugal tube and a beaker; ③, adding organic solvent; 40ml of acetone is added to the liquid A, and 40ml of acetone is also added to the remaining residue B to obtain a solid-liquid mixture C; ④, organic solvent extraction; the liquid A added with the organic solvent is allowed to stand for 1h. A dispersing agent is added to the obtained solid-liquid mixture C. After 40ml of ethylene glycol is added, stirring is conducted for 25min. After stirring, 5ml of ethylenediamine is added. Heating and stirring are conducted for 70min. The heating and stirring temperature is 70℃, and the stirring speed is 25r / min; ⑤, collecting filtrate: centrifugal treatment is conducted on the liquid in the centrifugal tube, and the supernatant D is collected. The solid-liquid mixture in the beaker is naturally cooled to room temperature, and the supernatant is obtained by standing. The supernatant E is collected. The supernatant D and the supernatant E are respectively detected and treated, and the supernatant is collected. The essence is obtained by standing.

[0032] Comparative Example 1 The same milk product in Example 1 is selected. Organic solvent is directly added, and extraction is conducted to extract the obtained liquid for detection.

[0033] Comparative Example 2 The same fruit and vegetable product in Example 1 is selected. After being squeezed and pressed, the obtained liquid is directly added with organic solvent, and extraction is conducted to extract the obtained liquid for detection.

[0034] Comparative Example 3 The same meat and fruit product in Example 1 is selected. After being crushed and mixed with water and being pressed, the obtained liquid is directly added with organic solvent, and extraction is conducted to extract the obtained liquid for detection.

[0035] The organic phosphorus residues of the above-mentioned examples 1 / 2 / 3 and comparative examples 1 / 2 / 3 were detected by using a gas chromatograph, the approximate value of the whole organic phosphorus was obtained by analyzing the amount of phosphorus element, and the mass ratio with the original sample was calculated to obtain the following table:

[0036] From the above table, for the same sample, after different sample pretreatment methods, the organic phosphorus residue obtained by using the method of the present application is higher than that obtained by using the traditional organic phosphorus detection method, so the detection pretreatment method provided by the present application is more effective and complete in extracting the residual organic phosphorus in fruits.

[0037] It should be noted that, in this document, relational terms such as first and second and the like can be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises", "comprising", or any other variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but can include other elements not expressly listed or inherent to such process, method, article, or apparatus. An element proceeded by "comprises... a" does not, without more constraints, exclude the existence of additional identical elements in the process, method, article, or apparatus that comprises the element.

[0038] The above description is only used to explain the technical solutions of the present application, not to limit the present application. Other modifications or equivalent replacements to the technical solutions of the present application made by those skilled in the art should be covered in the scope of claims of the present application.

Claims

1. A method for extracting fruit flavoring, characterized in that, Includes the following steps: ① Extract fruit samples; extract 5-15g from any part of the fruit, add deionized water for soaking (volume of deionized water is 30-45ml), soak for 1-2 hours, and use an ultrasonic instrument to perform ultrasound during the soaking process; ② Sample crushing; After soaking, the sample is mechanically crushed and pressed, and the resulting liquid A and residual residue B are collected and placed into centrifuge tubes and beakers respectively. ③ Add organic solvent; add organic solvent to liquid A, and add the same organic solvent to the remaining residue B to obtain solid-liquid mixture C; ④ Organic solvent extraction: Let the liquid A containing organic solvent stand for 1-2 hours. Add a dispersant to the resulting solid-liquid mixture C. After the dispersant is added, stir for 25-35 minutes. After stirring, add an alkaline additive and heat and stir for 60-85 minutes. ⑤ Collection of filtrate: Centrifuge the liquid in the centrifuge tube and collect the supernatant D. Let the solid-liquid mixture in the beaker cool naturally to room temperature and stand to obtain the supernatant E. Collect the supernatant D and supernatant E separately for testing and processing, and collect the supernatant. Let stand to obtain the fragrance.

2. The method for extracting fruit flavoring according to claim 1, characterized in that: In step ③, the organic solvents used include benzene, acetone, diethyl ether, chloroform, etc.

3. The method for extracting fruit flavoring according to claim 2, characterized in that: The volume ratio of the organic solvent to the deionized water is 1:1 to 1.

5.

4. The method for extracting fruit flavoring according to claim 1, characterized in that: The dispersant used in step ④ is either ethylene glycol or methanol.

5. The method for extracting fruit flavoring according to claim 4, characterized in that: The volume ratio of the dispersant to the deionized water is 1:1 to 1.

5.

6. The method for extracting fruit flavoring according to claim 1, characterized in that: The alkaline additive in step ④ is any one of polypyrrolidone, ethylenediamine, or sodium acetate.

7. The method for extracting fruit flavoring according to claim 6, characterized in that: The volume ratio of the liquid alkaline additive to the deionized water is 1:5-6, and the solid alkaline additive is 3-5g.

8. The method for extracting fruit flavoring according to claim 1, characterized in that: In step ④, the heating and stirring temperature is 60-75℃, and the stirring speed is 25-35 r / min.

9. The method for extracting fruit flavoring according to claim 3, characterized in that: In step 5, the supernatant D and supernatant E are obtained. When the fruit is in a liquid state, only supernatant D is taken. When the fruit is in a solid state, supernatant D and supernatant E are tested separately.

10. The method for extracting fruit flavoring according to claim 1, characterized in that: It also includes distillation, which includes the following steps: ① Extract fruit samples; extract 5-15g from any part of the fruit, add deionized water for soaking (volume of deionized water is 30-45ml), soak for 1-2 hours, and use an ultrasonic instrument to perform ultrasound during the soaking process; ② Sample crushing; After soaking, the sample is mechanically crushed and pressed, and the resulting liquid A and residual residue B are collected and placed into centrifuge tubes and beakers respectively. ③ Add organic solvent; add organic solvent to liquid A, and add the same organic solvent to the remaining residue B to obtain solid-liquid mixture C; ④ Organic solvent extraction: Let the liquid A containing organic solvent stand for 1-2 hours. Add a dispersant to the resulting solid-liquid mixture C. After the dispersant is added, stir for 25-35 minutes. After stirring, add an alkaline additive and heat and stir for 60-85 minutes. ⑤ Collection of filtrate: Centrifuge the liquid in the centrifuge tube and collect the supernatant D. Let the solid-liquid mixture in the beaker cool naturally to room temperature and stand to obtain the supernatant E. Collect the supernatant D and the supernatant E respectively for testing and processing. ⑥ Select the upper clear liquid D and upper clear liquid E after testing. Select the upper clear liquid with a higher organic content for distillation. Collect the distilled liquid and let it stand to obtain the fragrance.

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