CN116675598A - Method for preparing natural benzaldehyde from green calyx plums - Google Patents
Method for preparing natural benzaldehyde from green calyx plums Download PDFInfo
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- CN116675598A CN116675598A CN202310663056.4A CN202310663056A CN116675598A CN 116675598 A CN116675598 A CN 116675598A CN 202310663056 A CN202310663056 A CN 202310663056A CN 116675598 A CN116675598 A CN 116675598A
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- green calyx
- benzaldehyde
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- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 241001164374 Calyx Species 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 30
- 235000021018 plums Nutrition 0.000 title claims abstract description 30
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000007710 freezing Methods 0.000 claims abstract description 14
- 230000008014 freezing Effects 0.000 claims abstract description 13
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000006228 supernatant Substances 0.000 claims abstract description 8
- 239000002274 desiccant Substances 0.000 claims abstract description 5
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000012528 membrane Substances 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 2
- 229940095564 anhydrous calcium sulfate Drugs 0.000 claims description 2
- 239000012982 microporous membrane Substances 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 238000010025 steaming Methods 0.000 claims 1
- 235000019640 taste Nutrition 0.000 abstract description 8
- 239000003814 drug Substances 0.000 abstract description 6
- 229940079593 drug Drugs 0.000 abstract description 5
- 239000006227 byproduct Substances 0.000 abstract description 4
- 241001122767 Theaceae Species 0.000 abstract 1
- 239000003205 fragrance Substances 0.000 description 7
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 6
- 239000000284 extract Substances 0.000 description 5
- 244000018795 Prunus mume Species 0.000 description 4
- 235000011158 Prunus mume Nutrition 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 244000269722 Thea sinensis Species 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000004108 freeze drying Methods 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 description 2
- 244000144725 Amygdalus communis Species 0.000 description 2
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 description 2
- 241000122205 Chamaeleonidae Species 0.000 description 2
- 206010013911 Dysgeusia Diseases 0.000 description 2
- OVSQVDMCBVZWGM-SJWGPRHPSA-N Hyperin Natural products O[C@H]1[C@H](O)[C@@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-SJWGPRHPSA-N 0.000 description 2
- FVQOMEDMFUMIMO-UHFFFAOYSA-N Hyperosid Natural products OC1C(O)C(O)C(CO)OC1OC1C(=O)C2=C(O)C=C(O)C=C2OC1C1=CC=C(O)C(O)=C1 FVQOMEDMFUMIMO-UHFFFAOYSA-N 0.000 description 2
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 description 2
- 244000064622 Physalis edulis Species 0.000 description 2
- 235000003893 Prunus dulcis var amara Nutrition 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- QUKGYYKBILRGFE-UHFFFAOYSA-N benzyl acetate Chemical compound CC(=O)OCC1=CC=CC=C1 QUKGYYKBILRGFE-UHFFFAOYSA-N 0.000 description 2
- 235000019445 benzyl alcohol Nutrition 0.000 description 2
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 description 2
- 229940074393 chlorogenic acid Drugs 0.000 description 2
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 description 2
- 235000001368 chlorogenic acid Nutrition 0.000 description 2
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- QPJVMBTYPHYUOC-UHFFFAOYSA-N methyl benzoate Chemical compound COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- OVSQVDMCBVZWGM-DTGCRPNFSA-N quercetin 3-O-beta-D-galactopyranoside Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-DTGCRPNFSA-N 0.000 description 2
- BBFYUPYFXSSMNV-UHFFFAOYSA-N quercetin-7-o-galactoside Natural products OC1C(O)C(O)C(CO)OC1OC1=CC(O)=C2C(=O)C(O)=C(C=3C=C(O)C(O)=CC=3)OC2=C1 BBFYUPYFXSSMNV-UHFFFAOYSA-N 0.000 description 2
- 235000003840 Amygdalus nana Nutrition 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 235000010254 Jasminum officinale Nutrition 0.000 description 1
- 240000005385 Jasminum sambac Species 0.000 description 1
- 241000220299 Prunus Species 0.000 description 1
- 235000011432 Prunus Nutrition 0.000 description 1
- 235000004789 Rosa xanthina Nutrition 0.000 description 1
- 241000220222 Rosaceae Species 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- -1 aromatic aldehyde compound Chemical class 0.000 description 1
- 235000019606 astringent taste Nutrition 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 229940007550 benzyl acetate Drugs 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229940095102 methyl benzoate Drugs 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 235000014774 prunus Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000019600 saltiness Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/786—Separation; Purification; Stabilisation; Use of additives by membrane separation process, e.g. pervaporation, perstraction, reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/80—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Preparation Of Fruits And Vegetables (AREA)
Abstract
The invention discloses a method for preparing natural benzaldehyde from green calyx plums, which comprises the following steps: s1, picking fresh green calyx plums; s2, weighing a green calyx plum sample, pre-freezing, and performing vacuum freeze drying on the sample after the pre-freezing is completed; s3, performing S3; extracting the extracting solution in the freeze well in the vacuum freeze drying process by using an extracting agent, extracting the extracting solution by using an extracting agent, adding excessive drying agent into the extracting solution of the upper layer extracting agent, preserving in a refrigerator for 12 hours, extracting supernatant, filtering the supernatant by using a microporous filter membrane to obtain a mixed solution, and performing rotary evaporation on the mixed solution to obtain benzaldehyde. The method for preparing the natural benzaldehyde from the green calyx plums has the advantages that the taste of the green calyx plums is better after the benzaldehyde is extracted, the green calyx plums are not affected to be used as medicines and scented tea, the flower shape and the color are better, and the extraction of the benzaldehyde can be used as a comprehensive utilization of byproducts.
Description
Technical Field
The invention relates to the technical field of benzaldehyde extraction, in particular to a method for preparing natural benzaldehyde from green calyx plums.
Background
Benzaldehyde is the simplest aromatic aldehyde compound, is colorless or light yellow viscous liquid with bitter almond taste at normal temperature, is slightly soluble in water, and is mixed with organic solvent in any proportion. Benzaldehyde is an important fine chemical intermediate organic industrial raw material and is widely applied to the fields of medicines, dyes, fragrances, foods and the like.
The industrial production of benzaldehyde by toluene side-chain chlorination hydrolysis is the earliest, the process flow is long, the product separation is difficult, and meanwhile, organic wastes and corrosive gases are discharged, so that the environment is seriously polluted. More importantly, the produced benzaldehyde contains chlorine, so that the use of the benzaldehyde is greatly limited.
The current industrial technologies are toluene direct oxidation, styrene oxidation, benzoic acid or methyl benzoate reduction, benzyl alcohol oxidation, etc., and these chemical methods are all contaminated. The use of industrial products in the fields of medicine, perfume, food, etc. is limited.
Disclosure of Invention
The invention aims to provide a method for preparing natural benzaldehyde from green calyx plums, which has better taste after extracting the benzaldehyde, does not influence the use of the green calyx plums as medicines and scented tea, is better in flower type and color, and can comprehensively utilize the extracting of the benzaldehyde as a byproduct.
To achieve the above object, the present invention provides a method for preparing natural benzaldehyde from Prunus mume, comprising the steps of:
s1, picking fresh green calyx plums;
s2, weighing a green calyx plum sample, pre-freezing, and performing vacuum freeze drying on the sample after the pre-freezing is completed;
s3, performing S3; extracting the extracting solution in the freeze well in the vacuum freeze drying process by using an extracting agent, extracting the extracting solution by using an extracting agent, adding excessive drying agent into the extracting solution of the upper layer extracting agent, preserving in a refrigerator for 12 hours, extracting supernatant, filtering the supernatant by using a microporous filter membrane to obtain a mixed solution, and performing rotary evaporation on the mixed solution to obtain benzaldehyde.
Preferably, in step S1, picking fresh calyx Seu fructus Physalis as a bud of the selected calyx Seu fructus Physalis.
Preferably, in the step S2, the pre-freezing temperature of the green calyx plum sample is-18 to-40 ℃ and the pre-freezing time is 30min.
Preferably, in step S2, the temperature of vacuum freeze drying is-80 ℃ and the drying time is 48 hours.
Preferably, in step S3, the extraction liquid in the freeze well during the vacuum freeze drying is extracted with an extractant such that 7ml of extractant is added per 3ml of extraction liquid.
Preferably, in step S3, the temperature stored in the refrigerator is-18 ℃.
Preferably, in step S3, the thickness of the microporous membrane is 0.22. Mu.m.
Preferably, in step S3, the temperature of the rotary evaporation is 60-90 ℃.
Preferably, in step S3, the extractant is one of n-hexane, petroleum ether, methanol, and chloroform; the drying agent is one of anhydrous sodium sulfate, anhydrous calcium sulfate and anhydrous magnesium sulfate.
Therefore, the method for preparing the natural benzaldehyde from the green calyx plums has the following technical effects:
(1) The invention extracts benzaldehyde from natural green calyx plums, does not influence chlorogenic acid, hyperin, chameleon and the like which are taken as main medicinal components in the green calyx plums, has better taste after extracting the benzaldehyde, does not influence the green calyx plums which are taken as medicines and scented tea, and has better appearance in flower type and color.
(2) The extraction of benzaldehyde can be used as a by-product for comprehensive utilization.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a flow chart of a method of the present invention for preparing natural benzaldehyde from Prunus mume.
Detailed Description
The technical scheme of the invention is further described below through the attached drawings and the embodiments.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art. Such other embodiments are also within the scope of the present invention.
It should also be understood that the above-mentioned embodiments are only for explaining the present invention, the protection scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the protection scope of the present invention by equally replacing or changing the technical scheme and the inventive concept thereof within the scope of the present invention.
Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but are intended to be considered part of the specification where appropriate.
The disclosures of the prior art documents cited in the present specification are incorporated by reference in their entirety into the present invention and are therefore part of the present disclosure.
Example 1
The Prunus mume is Prunus mume belonging to Prunus of Rosaceae. The medicinal plum blossom recorded in the 2020 edition of Chinese pharmacopoeia comprises red plum blossom and white plum blossom, wherein the calyx of the plum blossom is in a grey green color, and the petals of the plum blossom are in a yellow-white color, which is also called green calyx plum, and the calyx green flower is in a white color and commonly called green plum.
Fig. 1 is a flowchart of a method for extracting benzaldehyde from green calyx plums, specifically as follows,
(1) Picking fresh green calyx plums, selecting bud parts of the green calyx plums, and weighing 50g of bud samples.
(2) Pre-freezing the bud sample, setting the pre-freezing temperature to be-18 ℃, and performing pre-freezing for 30min in a refrigerator.
When the buds reach-18 ℃, after the pre-freezing is finished, placing the pre-frozen bud samples on a freeze-drying plate of a vacuum freeze dryer, setting the temperature of a condenser at-80 ℃ and drying for 48 hours.
(3) And (3) taking out the extract in the freeze well of the freeze dryer in the vacuum freeze drying process, wherein the amount of the extract is 6ml, extracting with 14ml of n-hexane, and taking the upper n-hexane leaching solution after the extraction. Adding excessive anhydrous sodium sulfate into n-hexane leaching solution, removing water in leaching solution, storing the obtained solution in a refrigerator at-18deg.C for 12 hr, layering the solution, and extracting supernatant. Filtering the supernatant with a 0.22 mu m microporous filter membrane to obtain a mixed solution, and performing rotary evaporation on the mixed solution at the temperature of 70 ℃ to obtain benzaldehyde.
In order to verify that the method provided by the invention can efficiently extract benzaldehyde, GC-MS detection is carried out on the extracted benzaldehyde.
GC conditions: the column was DB-5MS (30 m. Times.0.25 mm. Times.0.25 μm); helium with high purity is used as carrier gas; the column flow rate is 1.0mL/min; the temperature is raised to the initial temperature of 40 ℃ for 2min, and then is raised to 250 ℃ for 15min at 5 ℃/min; the temperature of the sample inlet is 250 ℃, and the split sample is introduced.
MS conditions: an EI ion source, the ion source temperature being 230 ℃; the ionization voltage is 70eV, and the scanning range is 45-450 m/z.
The test results are shown in Table 1.
TABLE 1GC-MS detection results
As shown in Table 1, benzaldehyde was 95.76% of the total content. The fragrance components of the green calyx plum are mainly alcohols, aldehydes and lipid substances, the three volatile fragrance substances are flower and fruit fragrance, wherein the benzyl alcohol with rich content has weak fragrance, the benzaldehyde has obvious bitter almond taste, and the benzyl acetate is jasmine fragrance, so that the important components of the green calyx plum fragrance are formed, and especially the content of the benzaldehyde is relatively high. The content of aldehydes, especially benzaldehyde, in the volatile components after freeze-drying is high.
In order to verify the taste of the green calyx plum after extracting benzaldehyde by the method provided by the invention. Control and test groups were set for electronic tongue detection. The control group is green calyx plum which is not subjected to freeze drying treatment, 3g of green calyx plum is weighed, 150ml of boiling water is poured into the green calyx plum, after soaking is carried out for 8min, the soup is dripped into an evaluation bowl for summarization, and the green calyx plum is cooled to room temperature for detection. The test group uses 6.5ml of the freeze-dried extract of the present invention and 80ml of plain boiled water added to room temperature, and the solution was transferred into a measuring cup for measurement. The test group and the control group are detected for 4 times, and the data of the last 3 times are taken as output data. The results are shown in Table 2.
Table 2 taste index of test and control groups
| Sourness | Bitterness | Astringency | Aftertaste-B | Aftertaste-A | Umami | Richness | Saltiness | |
| Control group | -23.73 | 1.22 | -5.43 | 0.32 | 0.04 | 10.03 | 0.76 | 12.3 |
| Control group | -24.07 | 1.06 | -5.59 | 0.18 | -0.06 | 10.22 | 0.65 | 12.17 |
| Control group | -24.25 | 0.81 | -5.83 | 0.12 | -0.03 | 10.28 | 0.75 | 11.92 |
| ave | -24.02 | 1.03 | -5.62 | 0.21 | -0.02 | 10.18 | 0.72 | 12.13 |
| Test group | -15.65 | -0.06 | 2.86 | -0.59 | -0.04 | 5.54 | -0.1 | -3.3 |
| Test group | -15.38 | -0.61 | 2.78 | -0.57 | 0 | 5.4 | -0.07 | -4.03 |
| Test group | -15.4 | -1.04 | 2.76 | -0.62 | -0.03 | 5.28 | 0.1 | -4.36 |
| ave | -15.48 | -0.57 | 2.8 | -0.59 | -0.02 | 5.41 | -0.02 | -3.9 |
Therefore, the method for preparing the natural benzaldehyde from the green calyx plums is adopted, the benzaldehyde is extracted from natural plants, chlorogenic acid, hyperin, chameleon and the like which are taken as main medicinal components in the green calyx plums are not influenced, the taste of the green calyx plums after the benzaldehyde is extracted is better, the green calyx plums are not influenced to be taken as medicines and scented tea, and the flower type and the color are better; the extraction of benzaldehyde can be used as a by-product for comprehensive utilization.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (9)
1. A method for preparing natural benzaldehyde from green calyx plums, which is characterized by comprising the following steps:
s1, picking fresh green calyx plums;
s2, weighing a green calyx plum sample, pre-freezing, and performing vacuum freeze drying on the sample after the pre-freezing is completed;
s3, performing S3; extracting the extracting solution in the freeze well in the vacuum freeze drying process by using an extracting agent, extracting the extracting solution by using an extracting agent, adding excessive drying agent into the extracting solution of the upper layer extracting agent, preserving in a refrigerator for 12 hours, extracting supernatant, filtering the supernatant by using a microporous filter membrane to obtain a mixed solution, and performing rotary evaporation on the mixed solution to obtain benzaldehyde.
2. The method for preparing natural benzaldehyde from green calyx plums according to claim 1, wherein in step S1, fresh green calyx plums are picked as buds of green calyx plums.
3. The method for preparing natural benzaldehyde from green calyx plums according to claim 1, wherein the pre-freezing temperature of the green calyx plums in step S2 is-18 to-40 ℃ and the pre-freezing time is 30min.
4. The method for preparing natural benzaldehyde from green calyx plum according to claim 1, wherein in step S2, the temperature of vacuum freeze-drying is-80 ℃ and the drying time is 48h.
5. The method for preparing natural benzaldehyde from green calyx plum according to claim 1, wherein in step S3, the extraction liquid in the freeze well during vacuum freeze drying is extracted with an extractant in an amount of 7ml of extractant per 3ml of extraction liquid.
6. The method for preparing natural benzaldehyde from green calyx plum according to claim 1, wherein the temperature stored in the refrigerator in step S3 is-18 ℃.
7. The method for preparing natural benzaldehyde from green calyx plum according to claim 1, wherein the microporous membrane has a thickness of 0.22 μm in step S3.
8. The method for preparing natural benzaldehyde from green calyx plum according to claim 1, wherein the temperature of rotary steaming in step S3 is 60 to 90 ℃.
9. The method for preparing natural benzaldehyde from green calyx plums according to claim 1, wherein in step S3, the extractant is one of n-hexane, petroleum ether, methanol and chloroform; the drying agent is one of anhydrous sodium sulfate, anhydrous calcium sulfate and anhydrous magnesium sulfate.
Priority Applications (1)
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| JP2016128434A (en) * | 2015-01-06 | 2016-07-14 | Ｓｈｉｏｄａライフサイエンス株式会社 | Production method of natural benzaldehyde water, natural benzaldehyde water produced by production method, and antitumor agent containing natural benzaldehyde water |
| CN107879913A (en) * | 2017-11-09 | 2018-04-06 | 鹰潭华宝香精有限公司 | The preparation method of natural benzaldehyde |
| KR20230019559A (en) * | 2021-08-02 | 2023-02-09 | 한국식품연구원 | Natural aroma composition using citrus flower and manufacturing method thereof |
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| JP2016128434A (en) * | 2015-01-06 | 2016-07-14 | Ｓｈｉｏｄａライフサイエンス株式会社 | Production method of natural benzaldehyde water, natural benzaldehyde water produced by production method, and antitumor agent containing natural benzaldehyde water |
| CN107879913A (en) * | 2017-11-09 | 2018-04-06 | 鹰潭华宝香精有限公司 | The preparation method of natural benzaldehyde |
| KR20230019559A (en) * | 2021-08-02 | 2023-02-09 | 한국식품연구원 | Natural aroma composition using citrus flower and manufacturing method thereof |
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| Title |
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| 李雪玲等: "桃仁中苯甲醛的提取及其抑菌作用研究", 《生物学杂志》, vol. 27, no. 03, pages 423 - 424 * |
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