CN116869884A - Composition containing lemon peel extract and preparation method and application thereof - Google Patents
Composition containing lemon peel extract and preparation method and application thereof Download PDFInfo
- Publication number
- CN116869884A CN116869884A CN202310878588.XA CN202310878588A CN116869884A CN 116869884 A CN116869884 A CN 116869884A CN 202310878588 A CN202310878588 A CN 202310878588A CN 116869884 A CN116869884 A CN 116869884A
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- Prior art keywords
- lemon
- extract
- lemon peel
- oil
- peel extract
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
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- A61P37/08—Antiallergic agents
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- A—HUMAN NECESSITIES
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- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
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- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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Abstract
The invention discloses a composition containing lemon peel extract, which consists of lemon peel extract, 1, 2-hexanediol, 1, 2-pentanediol, propylene glycol and polyoxyethylene hydrogenated castor oil, wherein the lemon peel extract consists of lemon essential oil, lemon extract and lemon absolute oil. The fragrance of the composition has the characteristics of natural softness, plumpness and long duration, the lemon essential oil has fresh and soft head fragrance, the lemon extract has plumpness, smoothness and long duration, the cooperation of the lemon essential oil, the lemon essential oil and the lemon oil satisfies the characteristics of front, middle and rear and uniform fragrance, and the composition has the function of perfuming cosmetics. The lemon essential oil, the lemon extract and the lemon absolute oil all contain rich functional components, so that the composition provided by the invention has the characteristics of resisting bacteria, resisting oxidation, resisting inflammation, whitening and the like in different degrees; 1, 2-hexanediol, 1, 2-pentanediol and propylene glycol enhance the antibacterial and antiseptic functions of lemon peel extract, and have antibacterial and antiseptic effects for cosmetics.
Description
Technical Field
The invention relates to preparation and application of a composition containing rutaceae pericarp extract, in particular to a composition containing lemon pericarp extract, and a preparation method and application thereof.
Background
Synthetic essence perfume is generally used for perfuming in the existing cosmetics, and compared with natural essence perfume, the synthetic essence perfume has the fragrance of nature, softness and smoothness which are inferior to those of natural essence perfume, and most of synthetic essence perfume has no efficacy. Most cosmetics require the addition of preservatives to impart a certain shelf life to the cosmetics. The plant extract with natural fragrance, antiseptic effect and certain efficacy is developed to be used in cosmetics, accords with the natural development trend of the current cosmetics, and is more favored by consumers.
Lemon is the third largest variety in the citrus plants of the Rutaceae, is also a well-known fruit used as both medicine and food, and a great amount of lemon peel and other byproducts are produced in the eating and processing processes, and proved by modern pharmacological tests, the lemon peel has the pharmacological effects of resisting bacteria, diminishing inflammation, relieving asthma, eliminating phlegm, relieving cough, easing pain, promoting gastrointestinal motility, promoting digestive juice secretion and the like. The lemon peel is rich in volatile terpene, alkaloid, phenolic acid and other active ingredients, and the ingredients have attractive fragrance, antibacterial property and unique biological activity, can be applied to the field of beauty and skin care products, and can be used for replacing synthetic essence, resisting bacteria and preserving, and endowing cosmetics with special effects such as antioxidation (preventing skin aging), anti-inflammation (relieving, being not easy to be allergic), anti-tyrosinase (whitening), moisturizing and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a composition containing lemon peel extract with the effects of perfuming, antibiosis, antisepsis, antioxidation, antiallergic, whitening, moisturizing and the like, and a preparation method and application thereof.
The technical scheme adopted for solving the technical problems is as follows: a composition containing lemon peel extract comprises lemon peel extract, 1, 2-hexanediol, 1, 2-pentanediol, propylene glycol and polyoxyethylene hydrogenated castor oil according to (20-60): (10-20): (10-20): (10-20): the lemon peel extract consists of (10-20) lemon essential oil, lemon extract and lemon absolute oil according to the mass ratio of (20-60): (20-50): (20-30) by mass ratio.
The fragrance of the composition containing the lemon peel extract has the characteristics of natural softness, plumpness and long duration, the lemon essential oil has fresh and soft head fragrance, the lemon extract has plump and round fragrance, and the lemon absolute oil has long duration fragrance, and the matching of the three has the characteristics of front adjustment, middle adjustment and back adjustment of the fragrance and uniformity. The lemon peel extract not only has the effect of perfuming cosmetics, but also has the effects of resisting bacteria, resisting oxidation, resisting allergy, whitening, moisturizing and the like.
The lemon peel extracts of lemon essential oil, lemon extract and lemon absolute oil contained in the composition have antibacterial and antiseptic effects, and after the lemon peel extracts are combined with the three dihydric alcohols of 1, 2-hexanediol, 1, 2-pentanediol and propylene glycol according to a certain proportion, the antibacterial and antiseptic effects are enhanced, and the effect of antiseptic for cosmetics is achieved.
The polyoxyethylene hydrogenated castor oil is added into the composition disclosed by the invention, so that the components are uniformly mixed, the appearance of the product is uniform and is not layered, and the polyoxyethylene hydrogenated castor oil is more easily compatible with other raw materials of cosmetics.
We found through detection that:
1) 7 main compounds (relative percentage content > 1%) in the lemon essential oil account for 94.66% of total peak area, including D-limonene, beta-levopinene, gamma-terpinene and the like. The component with highest content is D-limonene (58.05%), has good antibacterial, antitussive, and expectorant effects, and can be used as raw material for preparing artificial neroli, sweet flower, lemon, bergamot oil, or as a fresh first fragrant perfume for use in cosmetic essence. Beta-levorotatory pinene (14.28%) is an important raw material for the perfume industry and for synthesizing other fine chemicals, has broad-spectrum antifungal effect, can inhibit the growth of a plurality of fungi, can be used for astringing skin, resisting depression, resisting cold, relieving distending pain and has a certain anticancer effect. Gamma-terpinene (11.98%) is a monoterpene, an orally effective antioxidant, can directly scavenge free radicals, can be used for pain relief, and has antifungal and anticoccidial properties.
2) The lemon extract contains 16 main compounds (relative percentage content > 1%) accounting for 92.96% of total peak area, including D-limonene, beta-bisabolene, alpha-bergamotene, etc. The highest content of D-limonene (22.95%). Beta-bisabolene (19.39%) is a component with fragrance and health care effects, has the fragrance of costustoot, citrus, flower, fruit, green and sweet balsam, and is widely used in the essence formulation of daily cosmetics; but also is a good antioxidant and has good antipruritic and anti-inflammatory functions. Alpha-bergamotene (accounting for 11.82%), also called bergapten, has high content in fingered citron, star anise and toona sinensis, and researches show that the alpha-bergamotene is a natural and effective anti-tumor medicament, and is frequently eaten and used by people both as a food seasoning ingredient and a natural medicament ingredient.
3) 7 main compounds (relative percentage content > 1%) in the lemon absolute comprise D-limonene, gamma-terpinene, beta-levorotatory pinene and the like, and account for 98.47% of the total peak area. Wherein D-limonene accounts for 63.79%, gamma-terpinene accounts for 18.82%, and beta-levopinene accounts for 5.13%.
4) The common components of lemon essential oil, lemon extract and lemon absolute oil are 7, namely beta-levopinene, myrcene, D-limonene, gamma-terpinene, citral, linalool and alpha-terpineol respectively. Citral, linalool and alpha-terpineol can be used as flavoring agent, lemon essence, etc., and also have antibacterial, antioxidant and antiinflammatory effects.
5) The components with the highest proportion in the three lemon peel extracts are terpene compounds (81.96% -96.64%). The oxygen-containing compounds such as alcohols, aldehydes and esters are also the main sources of aroma components of the lemon peel extract, and the relative contents of the oxygen-containing compounds in the three lemon peel extracts are as follows: lemon extract (17.8%) > lemon absolute (6.99%) > lemon essential (3.36%).
The preparation method of the composition containing the lemon peel extract comprises the steps of preparing lemon essential oil by adopting an enzymolysis steam distillation method, preparing lemon extract by adopting an ethanol leaching method, and preparing lemon absolute oil by adopting a petroleum ether leaching and alcohol precipitation method.
Specifically, the preparation process of the lemon essential oil comprises the following steps: weighing 100g of lemon peel in a round-bottom flask, adding 1000-3000 mL of distilled water, and adding sodium chloride accounting for 1-3% of the mass of the lemon peel and a cellulase mixture accounting for 1-2% of the mass of the lemon peel, wherein the cellulase mixture comprises cellulase with the enzyme activity of more than or equal to 1 ten thousand U/mg and hemicellulase with the enzyme activity of more than or equal to 1 ten thousand U/mg according to the following ratio of 2:1, the mass ratio of the components is 1; then adjusting pH value to 5-5.5 with citric acid, heating to 40-55 deg.C, hydrolyzing for 60-120 min, then raising temperature to keep micro-boiling reflux extraction until oil-free in distillate, separating by oil-water separator, collecting oily transparent liquid, drying with anhydrous sodium sulfate, storing in brown bottle, sealing, refrigerating at 4 deg.C for use. The prepared lemon essential oil is colorless transparent liquid, retains natural soft and fresh lemon fragrance, and has strong volatility.
Specifically, the preparation process of the lemon extract comprises the following steps: weighing 100g of lemon peel, adding 2-6% of propylene glycol and 300-600 mL of 90% ethanol by mass of the lemon peel, leaching for 2-3 times at 40-60 ℃ for 1-2 h, mixing the extracting solutions, standing, concentrating the supernatant under reduced pressure to remove the ethanol, storing the paste in a brown bottle for sealing, and refrigerating at 4 ℃ for later use. The prepared lemon extract is a yellow brown half paste, retains the peculiar fragrance of lemon, and has plump and mellow fragrance.
Specifically, the preparation process of the lemon absolute comprises the following steps: weighing 100g of lemon peel, adding 300-600 mL of petroleum ether, carrying out reflux extraction for 2-3 times at 40-60 ℃ for 1-2 h, combining the extracting solutions, standing, concentrating the supernatant under reduced pressure to paste, and mixing the supernatant with absolute ethyl alcohol according to a ratio of 1: mixing (5-10) by volume ratio, standing overnight at-20 ℃, collecting supernatant, concentrating under reduced pressure to remove solvent, storing in a brown bottle for sealing, and refrigerating at 4 ℃ for later use. The prepared lemon absolute oil is orange liquid, has longer and lasting smell than the lemon essential oil, and has better aroma and color than lemon extract.
Specifically, the preparation process of the composition containing the lemon peel extract comprises the following steps: weighing lemon essential oil, lemon extract and lemon absolute oil according to the following proportion (20-60): (20-50): mixing (20-30) by mass ratio to obtain lemon peel extract; taking 20-60 parts of lemon peel extract and 10-20 parts of polyoxyethylene hydrogenated castor oil, fully and uniformly stirring, then adding 10-20 parts of 1, 2-hexanediol, 10-20 parts of 1, 2-pentanediol and 10-20 parts of propylene glycol, and uniformly stirring.
The composition containing lemon peel extract can be used as flavoring agent, antiseptic, antibacterial agent, antioxidant, antiallergic agent (skin soothing agent), anti-tyrosinase agent (whitening agent) and humectant in cosmetics.
Compared with the prior art, the invention has the following advantages:
(1) the lemon peel extract provided by the invention has the characteristics of natural softness, smoothness and durability of the fragrance of the lemon essential oil, the lemon extract and the lemon absolute oil according to a certain proportion, the lemon essential oil is fresh and soft, the lemon extract is plump, the lemon absolute oil is long and durable, the matching of the lemon essential oil, the lemon extract and the lemon absolute oil meets the characteristics of front adjustment, middle adjustment and rear adjustment of the fragrance and is uniform, and the lemon peel extract has the function of perfuming cosmetics. The lemon peel extract of lemon essential oil, lemon extract and lemon absolute oil all contain rich functional components, so that the composition has the characteristics of resisting bacteria, resisting oxidation, resisting inflammation, whitening and the like in different degrees.
(2) The composition containing the lemon peel extract is added with the 1, 2-hexanediol, the 1, 2-pentanediol and the propylene glycol, so that the antibacterial and antiseptic functions of the lemon peel extract are enhanced, and the composition has the antibacterial and antiseptic effects on cosmetics.
(3) The addition of polyoxyethylene hydrogenated castor oil to the compositions of the present invention aids in the compatibility and uniform dispersion of the compositions of the present invention with other ingredients in the cosmetic.
(4) The composition containing the lemon peel extract can be used as an aroma agent, a preservative, an antibacterial agent, an antioxidant, an antiallergic agent, an anti-tyrosinase agent, a humectant and other functional agents in cosmetics such as skin lotion, skin cream and skin cream.
Drawings
FIG. 1 is a total ion flow chromatogram of three lemon peel extracts of the examples;
FIG. 2 is an electronic nose response value change of three lemon peel extracts in the examples;
figure 3 is a response curve of the maximum odor response values of three lemon peel extracts in the examples.
Detailed Description
The invention is described in further detail below with reference to the embodiments of the drawings.
1. The lemon peel extract in the composition containing the lemon peel extract is prepared from lemon essential oil, lemon extract and lemon absolute oil according to the following steps (20-60): (20-50): (20-30) by mass ratio.
The following are the preparation, evaluation and test results of three lemon peel extracts, namely lemon essential oil, lemon extract and lemon absolute oil:
(1) Preparation and sensory evaluation of three lemon peel extracts
Cleaning fresh lemon peel, removing white inner layer, drying at 40 deg.C for 1-3 hr, pulverizing, sieving with 8-16 mesh sieve, sealing with plastic bag, and storing.
Preparation of lemon essential oil: weighing 100g of lemon peel in a round-bottom flask, adding 1000-3000 mL of distilled water, and adding sodium chloride accounting for 1-3% of the mass of the lemon peel and a cellulase mixture accounting for 1-2% of the mass of the lemon peel, wherein the cellulase mixture comprises cellulase with the enzyme activity of more than or equal to 1 ten thousand U/mg and hemicellulase with the enzyme activity of more than or equal to 1 ten thousand U/mg according to the following ratio of 2:1, the mass ratio of the components is 1; then adjusting pH value to 5-5.5 with citric acid, heating to 40-55 deg.C, hydrolyzing for 60-120 min, then raising temperature to keep micro-boiling reflux extraction until oil-free in distillate, separating by oil-water separator, collecting oily transparent liquid, drying with anhydrous sodium sulfate, storing in brown bottle, sealing, refrigerating at 4 deg.C for use.
Preparation of lemon extract: weighing 100g of lemon peel, adding 2-6% of propylene glycol and 300-600 mL of 90% ethanol by mass of the lemon peel, leaching for 2-3 times at 40-60 ℃ for 1-2 h, mixing the extracting solutions, standing, concentrating the supernatant under reduced pressure to remove the ethanol, storing the yellow brown paste in a brown bottle for sealing, and refrigerating at 4 ℃ for later use.
Preparation of lemon absolute: weighing 100g of lemon peel, adding 300-600 mL of petroleum ether, carrying out reflux extraction for 2-3 times at 40-60 ℃ for 1-2 h, combining the extracting solutions, standing, concentrating the supernatant under reduced pressure to paste, and mixing the supernatant with absolute ethyl alcohol according to a ratio of 1: mixing (5-10) by volume ratio, standing overnight at-20 ℃, taking supernatant, concentrating under reduced pressure to remove solvent, storing orange-yellow liquid in a brown bottle for sealing, and refrigerating at 4 ℃ for later use.
Sensory quality comparisons of the three lemon peel extracts prepared are shown in table 1.
Table 1 sensory quality comparison of three lemon peel extracts
The lemon essential oil is colorless and transparent liquid, so that fresh lemon fragrance is reserved, and the volatility is high; the lemon extract is a yellow brown half paste, so that the naturalness of the lemon fragrance is maintained completely; the lemon absolute oil is orange liquid, has lasting and heavy smell compared with the lemon essential oil, and has better aroma and color than the lemon extract.
(2) GC/MS test of the three ingredients contained in the extracts of lemon peel
GC conditions: the capillary chromatographic column is HP-5MS elastic quartz capillary column (30 m×0.25mm×0.25 μm); the carrier gas is helium with the purity more than 99.999%; manual sample injection is adopted, and the split ratio is 200:1; the temperature of the sample inlet is 220 ℃; the temperature program was column Wen Chushi temperature 50 ℃ for 3min, 2 ℃/min to 110 ℃ for 10min, 2 ℃/min to 140 ℃ for 2min, 10 ℃/min to 250 ℃ for 5min (total 84min operation).
Mass spectrometry conditions: the ionization mode is electron bombardment ionization source (EI); the electron energy is 70eV; the transmission line temperature is 270 ℃; the ion source temperature is 230 ℃; delaying the solvent for 2min; scanning range is 35-550 u; the scanning mode is full scanning.
Analyzing the map by using NIST MS spectrum library, determining the name of each volatile substance, and calculating the relative content of each component by adopting an area normalization method.
The total ion flow chromatograms of the three lemon peel extracts are shown in figure 1. 22 chromatographic peaks are detected in total by the lemon essential oil, 39 chromatographic peaks are detected in total by the lemon extract, and 9 chromatographic peaks are detected in total by the lemon absolute oil.
The chemical compositions and relative percentages of the three lemon peel extracts are shown in table 2.
Table 2 chemical composition and relative percentage of three lemon peel extracts
Note that: "-" means a content of < 0.05 or undetected.
22 components are detected in the lemon essential oil, 7 compounds with the relative percentage content of more than 1 percent account for 94.66 percent of the total peak area, wherein the component with the highest content is D-limonene (58.05 percent), and the lemon essential oil has good effects of inhibiting bacteria, relieving cough, eliminating phlegm, relieving nervous tension, relieving pain, expelling toxin and beautifying, can be used as raw materials for preparing artificial orange flower, sweet flower, lemon and bergamot oil, and can also be used as a fresh first fragrant spice for being used in cosmetic essence. The beta-levorotatory pinene (14.28%) has resin and rosin aroma, is an important raw material for the perfume industry and synthesizing other fine chemicals, has broad-spectrum antifungal effect, can inhibit the growth of a plurality of fungi, can be used for astringing skin, resisting depression, resisting cold, relieving distending pain and has a certain anticancer effect. Gamma-terpinene (11.98%) is a monoterpene with citrus and lemon aromas, useful for formulating artificial lemon and peppermint essential oils; gamma-terpinene is also an orally effective antioxidant, can directly scavenge free radicals, can be used for pain relief, and has antifungal and anti-trypanosome properties.
39 components are detected in the lemon extract, 16 compounds with the relative percentage content of more than 1 percent account for 92.96 percent of the total peak area, wherein the highest content is 22.95 percent of D-limonene. Beta-bisabolene (19.39%) is a component with fragrance and health care effects, has the fragrance of costustoot, citrus, flower fragrance, fruit fragrance, green fragrance and sweet balsam, is widely applied to the essence formula of daily cosmetics, is a good antioxidant, and has good antipruritic and anti-inflammatory functions. Alpha-bergamotene (accounting for 11.82%), also called bergapten, has higher content in bergamot, star anise and toona sinensis, and researches show that the bergamotene is a natural and effective anti-tumor medicament, and is frequently eaten and used by people both as a food seasoning ingredient and a natural medicament ingredient.
The relative percentage of the lemon absolute oil is more than 1 percent and 7 types of the lemon absolute oil account for 98.47 percent of the total peak area, wherein D-limonene accounts for 63.79 percent, gamma-terpinene accounts for 18.82 percent, and beta-left-handed pinene accounts for 5.13 percent.
The component categories and the ratios of the three lemon peel extracts are shown in Table 3.
TABLE 3 component categories and ratios of three lemon peel extracts (%)
The components with the highest proportion in the three lemon peel extracts are terpene compounds (81.96% -96.64%). The oxygen-containing compounds such as alcohols, aldehydes and esters are also the main sources of aroma components of the lemon peel extract, and the relative content of the oxygen-containing compounds in the three lemon peel extracts is lemon extract (17.64 percent) > lemon absolute (6.99 percent) > lemon essential oil (3.36 percent) in sequence.
The common components of lemon essential oil, lemon extract and lemon absolute oil are 7, namely beta-levopinene, myrcene, D-limonene, gamma-terpinene, citral, linalool and alpha-terpineol respectively. Citral, linalool and alpha-terpineol can be used as flavoring agent, lemon essence, citrus flavor, etc., and have strong antibacterial, antioxidant and antiinflammatory activities. The components of the lemon peel extracts obtained by different extraction processes have certain similarity and difference, so that the three lemon peel extracts have coordination and complementation in the aspects of fragrance, functions and the like.
The comparison of the total flavonoids and total polyphenols of the three lemon peel extracts is shown in Table 4. The efficacy of flavone and polyphenol is various, belongs to strong antioxidant, can effectively remove free radicals in vivo, prevent cell degeneration and aging, inhibit exudation of inflammatory biological enzyme, promote wound healing and relieve pain, and can be used for various sensitive diseases.
TABLE 4 comparison of the total flavonoids and Total polyphenols of three lemon peel extractsn＝3)
(3) Electronic nose test analysis of three lemon peel extract odors
Three lemon peel extracts 2mL were precisely removed and equilibrated in a 10mL headspace bottle for 1min. And (3) detecting by using a PEN3 electronic nose at room temperature by adopting a headspace gas suction method. Measurement conditions: the sensor self-cleaning time is 150s, the sensor zeroing time is 5s, the sample preparation time is 5s, and the signal acquisition time is 300s. And analyzing the data by using WinMuster software matched with the PEN3 type sensor. The electronic nose response values of the three lemon peel extracts are shown in figure 2.
As can be seen from FIG. 2, the ten sensing elements all have different reaction intensities to the sample smell, and the response values are mainly concentrated on the S2, S7 and S9 probes. Wherein the essential oil and absolute oil have the highest response value S7, and the extract has the highest response value S2. As can be seen from tables 2 to 3, the terpene compounds are main components in the three lemon peel extracts, and the terpene compounds account for 96.64%, 81.96% and 93.01% of the essential oil, the extract and the absolute oil, respectively, so that the S7 response values of the essential oil and the absolute oil are relatively high. The extract contains the isocyanic compounds only, although the relative content is only 0.22%, and the response value of S2 is the highest, because the phenyl isothiocyanate has strong pungent smell and can be captured by the S2 probe even in extremely low concentration.
The response curve 3 was plotted according to the maximum response value, peaks of the odors of the three lemon peel extract samples were found, and the change in response value after reaching the peak value of 100s was measured, as shown in table 5.
Table 5 peak odour response and variation of three lemon peel extracts
Combining fig. 3 and table 5, the flavor intensity was judged from the maximum response peak: lemon essential oil (43.4134) > lemon extract (20.3461) > lemon absolute oil (16.6896), because the extract and absolute oil contain plant wax, pigment and the like besides terpenes and aromatic components, the sample viscosity is high, the aromatic components are difficult to break through the barrier, and the main reason is that the overall response value is low. According to the peak value and the corresponding G/G in the same time period after the peak value 0 The difference value between the values judges the fragrance retaining effect, three time periods are respectively 60s, 100s and 140s after the peak value, and the obtained fragrance durability is that: lemon absolute > lemon essential > lemon extract, which shows that the differences of the types and the contents of components of lemon peel extracts obtained by different extraction methods can influence the intensity, fullness and durability of fragrance.
Therefore, the aroma of the lemon essential oil is mainly enriched in the front section, and the richness is slightly poor; the lemon extract has rich and mellow fragrance, and the smell appears in the middle and rear sections; the lemon absolute has a strong fragrance but a good durability. The lemon extract can make up and link the intermediate aroma of the essential oil and the absolute oil, and the three are coordinated in aroma, multiple in level and capable of enhancing the durability of the aroma.
(4) In vitro antioxidant Activity assay of three lemon pericarp extracts
DPPH radical: 1mL of sample solution with different concentrations, 3mL of 1 mM/L of DPPH solution and 1mL of deionized water are added into a test tube according to the sequence until the total volume is 5mL, the sample solution is taken as a group to be tested, the sample solution is fully shaken uniformly and then reacts for 30min at normal temperature in a dark place, the sample solution is used for zeroing, and the absorbance A at 517nm is measured 1 . Using sample solution solvent to replace sample solution as blank group to measure A 0 . Absolute ethanol was used as a background group instead of DPPH solution to determine A 2 . Vitamin C was used as a positive control. Calculated according to the following example formula (1), the results are shown in Table 6.
ABTS radical: to the test tube, 1mL of sample solutions of different concentrations and 3mL of ABTS working solution (A 734nm 0.7+/-0.02) and 1mL of deionized water to a total volume of 5mL as a group to be measured, fully shaking up, performing light-shielding reaction at normal temperature for 30min, using a sample solution solvent as zeroing, and measuring the absorbance A at 734nm 1 . Using sample solution solvent to replace sample solution as blank group to measure A 0 . Absolute ethanol was used as a background group instead of ABTS solution to determine a 2 . Vitamin C was used as a positive control. Calculated according to the following example formula (1), and the calculated results are shown in Table 7.
TABLE 6 scavenging rate of DPPH free radical and IC by three lemon peel extracts 50 (n＝3)
From Table 6, it is clear that the DPPH radical scavenging ability of the three lemon peel extracts was enhanced with increasing concentration. The clearance of DPPH radicals is: lemon extract > lemon absolute > lemon essential. The clearance rate of the lemon extract with good effect on DPPH at 8mg/mL is up to 92.44 +/-1.99%.
TABLE 7 scavenging Rate and IC of three lemon pericarp extracts on ABTS free radical 50 (n＝3)
From Table 7, it can be seen that the ability of the three lemon peel extracts to scavenge ABTS free radicals increases with increasing concentration over the range of concentrations tested. The clearance of ABTS free radicals is: lemon absolute > lemon extract > lemon essential. The clearance rate of the lemon absolute oil to the ABTS free radical can reach 91.80+/-2.46% at the concentration of 0.7 mg/mL.
Three lemon peel extracts have differences in free radical scavenging effect, which is related to how much total flavonoids and total polyphenols are contained in the extract. From Table 5, it can be seen that the amount of total flavonoids and total polyphenols in lemon extract and absolute is greater than that in lemon essential. The flavone and polyphenol substances have better anti-free radical effect, and the rule of scavenging two free radicals generally coincides with the rule of changing the total flavone and total polyphenol content in the three extracts.
(5) In vitro anti-inflammatory Activity assay of three lemon pericarp extracts
The albumin inhibition assay was used for evaluation. Adding 0.4mL of fresh egg white diluent and 3.1mL of phosphate buffer solution (pH 6.8) into a test tube, fully shaking uniformly, adding 1.5mL of sample solutions with different concentrations until the total volume is 5mL, taking the sample solutions as a group to be tested, incubating in a water bath at 37 ℃ for 15min, immediately heating in a water bath at 70 ℃ for 10min, cooling, taking deionized water as a zeroing tube, and measuring the absorbance A at 660nm 1 . Measurement A was performed using PBS buffer as a blank instead of the sample solution 0 . PBS buffer solution is used as background group instead of egg white diluent, A is measured 2 . With ibuprofen (Standard)Drug) was used as a positive control. Calculated according to formula (2), the results are shown in Table 8.
Table 8 inhibition of albumin by three lemon peel extracts (%,n＝3)
from Table 8, it can be seen that, in the range of 5 to 200. Mu.g/mL of the test concentration, the three lemon peel extracts and the positive control ibuprofen each protect albumin from heat-induced damage to varying degrees and are concentration dependent, and the inhibition rates are: lemon absolute > lemon extract > lemon essential. The lemon absolute (200 mug/mL) with better effect shows an inhibition rate of 72.69+/-1.13%, which is comparable with ibuprofen. Studies have shown that limonene, linalool, alpha-pinene and the like have anti-inflammatory effects, and studies have also shown that beta-bisabolene has anti-inflammatory effects. Compared with the lemon absolute oil, the lemon absolute oil has the strongest anti-inflammatory effect.
(6) In vitro anti-tyrosinase activity assay for three lemon peel extracts
Sequentially adding the reagents in the sequence from top to bottom according to the table 9, shaking up thoroughly, incubating in a water bath at 37 ℃ for 10min, immediately adding tyrosine solution, keeping the temperature at 37 ℃ in a dark place for 30min, cooling, zeroing with deionized water, and measuring A of each group of samples 475nm . The tyrosinase inhibition rate was calculated according to formula (3) using arbutin as a positive control, and the results are shown in Table 10.
TABLE 9 reaction solution composition for measurement of tyrosinase inhibition ratio
Table 10 inhibition ratio and IC of three lemon peel extracts to tyrosinase 50 (n＝3)
As can be seen from table 10, the inhibition of tyrosinase activity by the three lemon peel extracts was all enhanced with increasing concentration, and the inhibition rate of tyrosinase was as follows: lemon essential oil > lemon extract > lemon absolute oil. The inhibition rate of the lemon essential oil can reach 93.82+/-1.06% when the concentration of the lemon essential oil is 20mg/mL, and is far higher than that of the positive control arbutin. And IC of three kinds of lemon peel extracts 50 The values are all lower than arbutin IC 50 The value of 29.40mg/mL indicates that the anti-tyrosinase effect of the bearberry extract is better than that of arbutin. The lemon peel is rich in various bioactive substances such as flavone, polyphenol and the like, and can be used as a substrate analogue to combine tyrosinase due to the fact that the bioactive substances are similar to the substrate structure of tyrosinase, so that the effect of inhibiting melanin generation is achieved; citral, neryl acetate, pinene, and the like are also major contributors to inhibition of tyrosinase activity; the synergistic effect of different compounds makes the extract have different degrees of inhibition effect on tyrosinase.
(7) Antimicrobial assay of three lemon peel extracts
Preparing strains to be tested: activating strain with MH culture medium, culturing Escherichia coli and Staphylococcus aureus at 37deg.C and Candida albicans at 28deg.C to logarithmic phase, centrifuging for 10min at 5000r/min, collecting precipitate, washing the precipitate with 0.9% sterile physiological saline for 2 times, re-suspending bacteria with MH culture medium, and adjusting concentration of bacterial liquid to 1×10 8 CFU/mL is the bacterial liquid to be detected.
Sample solution preparation: three lemon peel extracts were precisely weighed 0.100g each and dissolved in 1mL DMSO to give a 100mg/mL sample stock solution.
And (3) antibacterial rate measurement: the experiment is divided into a blank group, a solvent blank group and an experiment group, wherein the experiment group comprises a lemon essential oil group, an extract group and a clean oil group. Taking a sterile 96-well plate, and adding 170 mu L of MH culture medium and 30 mu L of bacteria liquid to be detected into a blank group; solvent blank was added with 200 μl MH medium containing samples of different concentrations; 170. Mu.L of MH medium containing the sample and 30. Mu.L of bacteria liquid to be tested are added to the experimental group. After incubation in an incubator for 18h, absorbance was measured at 600nm using an enzyme-labeled instrument. Three duplicate wells per sample.
The bacteriostasis rate is calculated according to formula (4), and the result is shown in Table 11.
Table 11 antibacterial ratio of three lemon peel extracts to escherichia coli, staphylococcus aureus and candida albicans (%,n＝3)
comparing the antibacterial performance of the three lemon peel extracts in Table 11, the antibacterial capability of the lemon essential oil with the same concentration is found to be stronger than that of the lemon extract and the lemon absolute oil, wherein the lemon extract and the lemon absolute oil are more sensitive to escherichia coli than staphylococcus aureus and candida albicans, and the antibacterial rate of the lemon extract and the lemon absolute oil to the three bacteria is more than 90% when the concentration is more than 12.5 mg/mL. At the concentration of 50mg/mL, the antibacterial rate of the three lemon peel extracts to three bacteria reaches more than 93 percent (except for the lemon extract to staphylococcus aureus).
2. The lemon peel extract contained in the composition of the invention comprises lemon essential oil, lemon extract and lemon absolute oil according to the following (20-60): (20-50): (20-30) by mass ratio. Based on the fact that three lemon peel extracts have advantages and differences in fragrance, free radical resistance, inflammation resistance, tyrosinase resistance and bacteria resistance, the lemon peel extract is specifically as follows:
(1) The fragrance, the fullness and the durability of the fragrance of the three are characterized, and can complement each other;
(2) DPPH resistance: lemon extract > lemon absolute > lemon essential;
(3) ABTS resistance: lemon absolute > lemon extract > lemon essential;
(4) Anti-inflammatory effects: lemon absolute > lemon extract > lemon essential;
(5) Anti-tyrosinase performance: lemon essential oil > lemon extract > lemon absolute oil;
(6) Antibacterial properties: the lemon essential oil is superior to the extract and the absolute oil.
Therefore, the invention prepares the three lemon peel extracts into a mixture according to a certain proportion so as to achieve the complementary enhancement effect.
Example 1: weighing 50 parts of lemon essential oil, 20 parts of lemon extract and 30 parts of lemon absolute oil, and uniformly mixing to obtain the lemon peel extract, wherein the color state of the lemon peel extract is yellow liquid, and the fragrance characteristic of the lemon extract is pure, fresh and plump and long. The anti-radical, anti-tyrosinase, antibacterial, anti-inflammatory experiments were performed as described above, and the results are shown in Table 12.
Table 12 inhibition (%) test results of lemon peel extract on related indexes [ (]n＝3)
Therefore, after the three lemon peel extracts are mixed according to a certain proportion, the fragrance and the efficacy of the lemon peel extracts have complementary enhancement effects, and the lemon peel extracts are more favorable for being used as a fragrance agent and an efficacy agent of cosmetics.
3. The composition containing the lemon peel extract comprises the lemon peel extract, 1, 2-hexanediol, 1, 2-pentanediol, propylene glycol and polyoxyethylene hydrogenated castor oil (such as PEG-40 hydrogenated castor oil) according to the following steps of (20-60): (10-20): (10-20): (10-20): (10-20) by mass ratio. Wherein the lemon peel extract is prepared from lemon essential oil, lemon extract and lemon absolute oil according to the following proportion (20-60): (20-50): (20-30) by mass ratio. The composition containing the lemon peel extract can be used as an additive for effective raw materials such as a flavoring agent, a preservative, an antibacterial agent, an antioxidant, an antiallergic agent, a whitening agent, a humectant, an anti-tyrosinase, a skin soothing agent and the like in cosmetics such as skin lotion, skin cream and the like.
(1) Example 2 and comparative example: formula and preparation of soft face cream
Formulation of the cream product of Table 12
Preparation of example 2: sequentially feeding the component A into an emulsifying pot, heating, stirring and heating to 80 ℃; mixing the component B, heating to 80 ℃, pouring the component B into the component A, and homogenizing and stirring for 15min under heat preservation. Continuously stirring and cooling to 45-50 ℃, adding the component C, continuously stirring for 15min, and discharging.
Preparation of comparative example: sequentially feeding the component A into an emulsifying pot, heating, stirring and heating to 80 ℃; mixing the component B and the component D, heating to 80 ℃, pouring the component B+D into the component A, and homogenizing and stirring for 15min under heat preservation. Continuously stirring and cooling to 45-50 ℃, adding the component E, uniformly mixing and discharging.
(2) Example 2 and comparative example: sensory, spreadability, stability and microbiological tests of the creams were compared according to cosmetic safety technical Specification (2015 edition, national drug administration, 2019, no. 40), and the test results are shown in tables 13 and 14.
Table 13 organoleptic indicators and stability of the cream products
50g of the cream products of example 2 and comparative example were placed in a bottle, covered and sealed, and after 10 days in a 40℃oven, samples were taken for microbial detection as follows:
table 14 microbiological test results of the cream products
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Claims (7)
1. A composition containing lemon peel extract, which is characterized in that the composition comprises lemon peel extract, 1, 2-hexanediol, 1, 2-pentanediol, propylene glycol and polyoxyethylene hydrogenated castor oil according to the following proportion (20-60): (10-20): (10-20): (10-20): the lemon peel extract consists of (10-20) lemon essential oil, lemon extract and lemon absolute oil according to the mass ratio of (20-60): (20-50): (20-30) by mass ratio.
2. The method for preparing the composition containing the lemon peel extract of claim 1, wherein the lemon essential oil is prepared by adopting an enzymolysis steam distillation method, the lemon extract is prepared by adopting an ethanol leaching method, and the lemon absolute oil is prepared by adopting a petroleum ether leaching and alcohol precipitation method.
3. The method of preparing a lemon peel extract-containing composition according to claim 2, wherein the preparation process of the lemon essential oil is as follows: weighing 100g of lemon peel in a round-bottom flask, adding 1000-3000 mL of distilled water, and adding sodium chloride accounting for 1-3% of the mass of the lemon peel and a cellulase mixture accounting for 1-2% of the mass of the lemon peel, wherein the cellulase mixture comprises cellulase with the enzyme activity of more than or equal to 1 ten thousand U/mg and hemicellulase with the enzyme activity of more than or equal to 1 ten thousand U/mg according to the following ratio of 2:1, the mass ratio of the components is 1; then adjusting the pH value to 5-5.5 by using citric acid, heating to 40-55 ℃ for enzymolysis for 60-120 min, then raising the temperature to keep micro-boiling reflux extraction until oil in the distillate is free of oil drops, collecting oily transparent liquid after separation by an oil-water separator, drying by using anhydrous sodium sulfate, and storing in a brown bottle for sealing.
4. The method of preparing a composition containing lemon peel extract according to claim 2, wherein the preparation process of the lemon extract is: weighing 100g of lemon peel, adding 2-6% of propylene glycol and 300-600 mL of 90% ethanol by mass of the lemon peel, leaching for 2-3 times at 40-60 ℃ for 1-2 h, mixing the extracting solutions, standing, concentrating the supernatant under reduced pressure to remove the ethanol, and storing the paste in a brown bottle for sealing.
5. The method of preparing a lemon peel extract-containing composition according to claim 2, wherein the preparation process of lemon absolute is: weighing 100g of lemon peel, adding 300-600 mL of petroleum ether, carrying out reflux extraction for 2-3 times at 40-60 ℃ for 1-2 h, combining the extracting solutions, standing, concentrating the supernatant under reduced pressure to paste, and mixing the supernatant with absolute ethyl alcohol according to a ratio of 1: mixing (5-10) by volume ratio, standing overnight at-20 ℃, collecting supernatant, concentrating under reduced pressure to remove solvent, and storing in a brown bottle for sealing.
6. The method of preparing a composition containing lemon peel extract according to claim 2, wherein the preparation process of the composition containing lemon peel extract is as follows: weighing lemon essential oil, lemon extract and lemon absolute oil according to the following proportion (20-60): (20-50): mixing (20-30) by mass ratio to obtain lemon peel extract; taking 20-60 parts of lemon peel extract and 10-20 parts of polyoxyethylene hydrogenated castor oil, fully and uniformly stirring, then adding 10-20 parts of 1, 2-hexanediol, 10-20 parts of 1, 2-pentanediol and 10-20 parts of propylene glycol, and uniformly stirring.
7. Use of the lemon peel extract containing composition of claim 1 as a fragrance, preservative, antibacterial, antioxidant, antiallergic, anti-tyrosinase agent, and humectant in cosmetics.
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| CN117224445B (en) * | 2023-10-20 | 2024-03-29 | 妆莱(广州)生化科技有限公司 | Perfume lemon type essential oil containing tree peony root bark extract and preparation process and application thereof |
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