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A method and device for extracting cinnamaldehyde-rich composition from cinnamon bark

A technology of cinnamaldehyde and cinnamon bark is applied in separation methods, chemical instruments and methods, solvent extraction and other directions, and can solve the problems of difficulty in separating essential oils, low cinnamaldehyde content, and difficulty in removing organic solvents completely.

Active Publication Date: 2021-03-09
三益创价生物科技(深圳)有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, CN201210518917.1, CN102964228B, CN102964229B, CN201210518899.7, CN201210518963.1, CN201220666255.8, CN201220666403.6 respectively utilize complex steam distillation equipment to extract cinnamaldehyde, to still not improve the yield, but the efficiency
[0004] Take the solvent extraction method as an example, for example: China Taiwan No. 401394 patent, with methanol, CH containing ether 2 N 2 Organic solvent extraction such as solution, and then chloroform distribution extraction; Chinese Taiwan No. I495487 patent, by being selected from ethanol, propylene glycol, 1,3-butanediol, chloroform, dichloroethane, carbon tetrachloride, acetone, One or two or more extraction solvents of ethyl acetate and hexane are used for extraction; China Taiwan Patent No. I549686 continuously extracts cinnamon with methanol, and after three consecutive extractions, methanol extract is obtained. The methanol extract uses Methanol, water and n-hexane are used for partition extraction; CN201710245493.9 uses n-hexane as a solvent to extract cinnamon; but the disadvantage of these organic solvent extraction methods is that it is difficult to completely remove harmful organic solvents after extraction
[0005] Taking the supercritical carbon dioxide extraction method as an example, for example: China Taiwan No. I352611 patent, extracts the fat-soluble essential oil components in the cinnamon leaf fragments with supercritical carbon dioxide; but the extract obtained by the supercritical carbon dioxide extraction method has a main component of Essential oil, cinnamaldehyde content is low, and it is not easy to separate from essential oil

Method used

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  • A method and device for extracting cinnamaldehyde-rich composition from cinnamon bark
  • A method and device for extracting cinnamaldehyde-rich composition from cinnamon bark
  • A method and device for extracting cinnamaldehyde-rich composition from cinnamon bark

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] Wash the blades of Cinnamomum Cassia, dried, then pulverized into a fragment of 1-10 mm.

[0082] 350 grams of jade leaves, poured into the extract of the subcritical propane fluid extraction device, and then sequentially: determining the path of the pu, extracting tank, separation tank, etc.; injection with propane storage tank isometric propane (8bar); Setting extraction conditions: propane flow 12 liters per hour, extracting groove pressure 45bar / temperature 60 ° C, separation tank pressure 8-10 bar / temperature 50 ° C. The propane subcritical extract was performed by the above conditions for 2 hours, 3.7 grams of product, and the GC-MS spectrum see figure 1 Among them, the main components: the cinnamolide content is about 42%, the extraction rate is 86.3% (3.7 x 0.2 / 1.8); secondary ingredient: o-methoxycinnamic aldehyde is about 11.2%, hard finger Methyl Stearates approximately 14.9%, COUMARIN is about 7.9%; other components see Table 1.

[0083] Table 1: Componen...

Embodiment 2～13

[0087] The class is also prepared for Example 1, but the subcritical extraction conditions are slightly different, see Table 2, the resulting product is also shown in Table 2 below. Among them, the GC-MS maps of Examples 8, 9, 12, 13 are respectively see figure 2 3, 4, 5, of which the cinnamon is about 36 ~ 42%, and the yield is about 2.5 to 3.5 g.

[0088] Table 2: Preparatory propane flow (L / HR), extraction tank pressure (BAR), and product weight (g) of Examples 1 to 13, extract temperature (° C).

[0089]

[0090] The main components of Examples 2 to 13, the secondary ingredients, and other detection ingredients, all of which are all kinds of preparation Examples 1, the proportion is also the same, figure 2 , 3, 4, 5, respectively figure 1 The comparison can be confirmed. Further, it is also prepared, and the calcinal solvent content is 36%, the yield 2.5; the preparation Example 9 cinnamide content is 39%, the yield is 2.7 g; the preparatory Example 12 cinnamon content ...

Embodiment 2

[0100] According to the preparation Example 1, the SPE extraction conditions were extracted with cinnamon, and the raw material was Yulipi, and 386 grams of cinnamon confection composition were obtained, and the alcohol of twice the weight of the cinnamide composition. Figure 9 The SFF extraction tank of the SFF device is 15 to 16 kg / h, the pressure is 100 bar, the temperature is 60 ° C, the temperature is 60 ° C; the carbon dioxide flow of the first SFF fractionation is 15 to 16 kg / hour, The pressure is 75 bar, the temperature is 60 ° C; the carbon dioxide flow of the second SFF fraction tank is 15 to 16 kg / h, the pressure is 50 bar, the temperature is 50 ° C; and the carbon dioxide flow of the third SFF fractionation is 15 to 16 kg. / Hours, the pressure is 45 bar, the temperature is supercritical fractionation under the conditions of 20 ° C, and the composition of 261 clinic aldehydrate can be extracted at the first SFF fractional tank. Its GC-MS map see Figure 8 . Each...

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Abstract

The invention discloses a method and a device for extracting a composition rich in cinnamaldehyde from cinnamon bark, and relates to the technical field of chemical extraction. The method comprises: washing, drying, and crushing cinnamon bark into fragments; pouring the cinnamon bark fragments into an SPE extraction tank of a subcritical propane fluid extraction device for subcritical propane fluid extraction; introducing the extraction fluid into an SPE separation tank; removing the SPE Separating the propane in the tank to obtain the cinnamaldehyde composition; the cinnamaldehyde composition is subjected to supercritical fractionation, wherein the supercritical fractionation hardware contains at least the SFF extraction tank, the first SFF fractionation tank, the second SFF fractionation tank and the third SFF fractionation tank; subcritical propane fluid extraction conditions are: SPE extraction tank pressure is 30-55 bar, temperature is 40-75 ° C; supercritical fractionation conditions are: SFF extraction tank pressure is 75-350 bar, temperature is 32-100 ° C The pressure of the first SFF fractionation tank is 74-250 bar, and the temperature is 32~100°C; the pressure of the second SFF fractionation tank is 45-200 bar, and the temperature is 32~100°C; and the pressure of the third SFF fractionation tank is 40-150 bar, temperature 5-100°C.

Description

Technical field [0001] The present invention relates to the field of chemical extraction techniques, and more particularly to a method of extracting a cinnamon-rich aldehyde composition from a cinnamon leather. Background technique [0002] Cinnamonal / leaf / leaf-containing calculating aldehyde, known extraction method, no ovidion, organic solvent extraction method, supercritical fluid extraction method. [0003] Take the water extraction as an example, for example, China Taiwan No. 09914436 patent application, which is extracted in a state of distilled water; China Taiwan No. 1163988 is patented, the secondary water is added to the temperature range of 180 ° C -220 ° C Boiled soil cinnamon leaves to obtain extracts; China Taiwan, Patent No. 1194117, continuously distilled with a water vapor distillation, and obtains aqua ingredients, CN201610660116.7 extracts with water vapor; Therefore, the method of extraction is not high, and the amount of cinnamonaldehyde is not high in th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D11/02B01D3/14
CPCB01D3/14B01D11/0203B01D11/0284B01D11/0288
Inventor 吴宇建蔡庆瑞林圣富林士闳卢士钧席美华吴靖苡吴鑫阳吴宣德
Owner 三益创价生物科技(深圳)有限公司
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