CN102002439B - Medicinal and edible plant chimonanthus grammatus essential oil, and preparation method and application thereof - Google Patents

Medicinal and edible plant chimonanthus grammatus essential oil, and preparation method and application thereof Download PDF

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CN102002439B
CN102002439B CN2010105479090A CN201010547909A CN102002439B CN 102002439 B CN102002439 B CN 102002439B CN 2010105479090 A CN2010105479090 A CN 2010105479090A CN 201010547909 A CN201010547909 A CN 201010547909A CN 102002439 B CN102002439 B CN 102002439B
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essential oil
wax plum
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CN102002439A (en
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朱笃
刘易鑫
张志斌
邹峥嵘
颜日明
曾庆桂
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Jiangxi Normal University
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Abstract

The invention relates to a medicinal and edible plant chimonanthus grammatus essential oil, and a preparation method and application thereof. The chimonanthus grammatus essential oil is extracted by a vapor distillation method; 53 components are detected by gas-phase chromatogram-mass spectrum combined technology; the identified components occupy 99.99 percent of total peak area of a chromatogram of volatile oil; and the main components of the essential oil are (E)-3-(4,8-dimethyl-3,7-nonene)-furan, acetyl borneol ester, 6,6-dimethyl-3-methylene-bicyclo[3.1.1] heptane, tetrahydro solasodine, ledene alcohol, 1,5-dimethyl-1-ethenyl-4-hexenyl butyrate and the like which account for 49.87 percent of the total components of the volatile oil. The essential oil has higher antibacterial activity, wider antibacterial spectrum and high anti-oxidation activity; and can be used as a natural antibacterial and antioxidant active ingredient for preparing cosmetic additives, food additives, medicinal products, health-care products and the like.

Description

The prominent holder of medicine food dual purpose plant wax plum essential oil and its production and use
Technical field
The present invention relates to the prominent holder of a kind of medicine food dual purpose plant wax plum essential oil preparation method and its usage, adopt extraction by steam distillation to separate essential oil, biological activity assay proves that this derived essential oil has well antibacterial and anti-oxidant activity, has the good purposes in fields such as being applied to cosmetics additive, foodstuff additive, medicinal and healthcare products.
Background technology
Microbial contamination is a major issue most threatening in makeup, foodstuffs industry always, it not only produces great effect in production and quality examination process, the more important thing is the consumer health is caused a significant threat, therefore, the interpolation of sanitas is inevitable.But due to the interpolation of a large amount of Chemical Preservatives, when anti-bacteria grew, its safety in utilization also existed very large query.Today that health demand is being strengthened day by day, the makeup and the related products thereof that use as Pursuit for Aesthetics, should reduce as much as possible it to human consumer's health threat, food safety is also a major issue of people's growing interest simultaneously, and therefore deriving from natural natural bacteriostatic composition is only the key point that addresses this problem.Plants essential oil is as a kind of active skull cap components, and its inherent fragrance and its various biological activitys that have are that it becomes the first-selection that addresses this problem.
Essential oil (Essential oils) claims again volatile oil (Volatile oils), be present in a class in plant have aromatic odour, can with wet distillation out and with the general name of the not miscible volatility oily composition of water.The interpolation that the interpolation that studies show that essential oil can effectively replace or reduce Chemical Preservative guarantees the validity of protective system simultaneously, many plants essential oils also possess the medicinal health effects such as anti-oxidant, anti-inflammatory, antiviral, antitumor, antipyretic-antalgic, expelling phlegm for arresting cough simultaneously in addition, and these activity make it give full play to its exclusive effect and progressively be approved by people from produce too many levels that the human consumer uses in makeup, foodstuffs industry.
Wax plum platymiscium is under the jurisdiction of Laurales, Calycanthaceae, and its ornamental value gets most of the attention in China always, and simultaneously, wax plum platymiscium is also China's traditional Chinese medicine, has high medicinal, edibleness.There are some researches prove in this platymiscium body and contained abundant bioactive ingredients, have relieving cough and reducing sputum, anti-inflammatory is analgesic, the pharmacological effect of antibiotic, anti-oxidant, antiviral, step-down, analgesia, strengthening immunity, its main active ingredient is essential oil, alkaloid and Flavonoid substances.Prominent holder wax plum is that the wax plum belongs to a novel species, is the domestic endemic species in Jiangxi, and because its areal distribution is narrow and small and rarely known by the people, its exploitation are in the starting stage, and it is blank that the natural radioactivity development of resources still belongs to.According to existing research method, derived essential oil has been carried out preliminary study, find that it has stronger bacteriostatic activity, wider antimicrobial spectrum and good anti-oxidant activity, show that this plant resources has unlimited potentiality to be exploited, be expected to become the natural bacteriostatic of makeup, foodstuff additive, medicinal and healthcare products etc., the new type resource of oxidation-resistant active ingredient.
Summary of the invention
The object of the invention is, preparation method and the purposes of the prominent holder of a kind of medicine food dual purpose plant wax plum essential oil are provided, by a series of pharmacology activity researchs, confirm that it has stronger bacteriostatic activity and anti-oxidant activity, can be used as the purposes of anticorrosion, the antioxidant addn of the series such as makeup and food.
It is simple that the present invention extracts the extracting method flow process, easy to operate, with low cost, and yield is high, safe and reliable, and substance environment pollutes, and products obtained therefrom has higher purity, is fit to the characteristics such as large production, is a kind of good extraction and separation method.
a kind of prominent holder of medicine food dual purpose plant wax plum essential oil that utilizes extraction by steam distillation of the present invention, choose prominent holder in autumn wax plum without the complete fresh leaf of scab, gather, clean, natural air drying, pulverize, wet distillation, oily water separation can obtain prominent holder wax plum essential oil, oil yield is 0.7-1.5%, its main chemical compositions is (E)-3-(4, 8-dimethyl-3, 7-nonene base)-furans 13.81%, acetyl norbornene ester 12.66%, 6, 6-dimethyl-3-methylene radical-dicyclo [3.1.1] heptane 7.06%, tetrahydrochysene solasodine 5.93%, loudspeaker enol 5.32%, 1, 5-dimethyl-1-vinyl-4 butyric acid hexene ester 5.09% composition such as grade, account for 49.87% of total volatile oil composition.This essential oil main component is olefines, wherein is mainly terpene substances, and wherein geranic acid, myrcene etc. are important spice source, and cadinol is promoting the important roles such as human body hormone secretion, the thyroid infiltration of raising.
The extracting method of the prominent holder of described medicine food dual purpose plant wax plum essential oil, its extraction step is:
(1) select the complete disease-free fresh blade of prominent holder wax plum in autumn, remove impurity, with flushing with clean water 1-3 time, natural air drying 12-48 hour, pulverize and sieve the 20-60 order, sealing saves backup;
(2) take a certain amount of prominent holder wax plum powder in round-bottomed flask, add water 5-10 and doubly measure, wet distillation 6-8 hour;
(3) distillate is loaded in separating funnel, standing 0.5 hour, reclaims the faint yellow transparent oily liquid in upper strata;
(4) remove moisture with anhydrous sodium sulfate drying, be prominent holder wax plum essential oil, yield is: 0.7%-1.5%, and in brown air-tight bottle-20 ℃ preservation.
Described prominent holder wax plum essential oil, very obvious to the fungistatic effect of the ten tested bacterium of strain, minimum inhibitory concentration and minimal bactericidal concentration are all between 2-16mg/ml.Simultaneously it carried out reductibility and remove free radical activity and detect, DPPH free radical scavenging activity IC 50=12.145mg/ml.Cosmetics preservative challenge test demonstration, this essential oil can play good sterilization and anticorrosion effect to three kinds of tested bacterium of inoculation within the test period.General performance is, this essential oil has broad-spectrum antibacterial effect and good anti-oxidant activity.
It is active and active than strong anti-oxidation that described prominent holder wax plum essential oil has good broad-spectrum antibacterial, this essential oil fragrance is pure and fresh pleasant, be suitable as very much cosmetics additive, the effect of its performance not only can be used as antipathogenic composition, also comprises the antidotal natural effective active composition of degerming.The present invention is lipotropy pale yellow oily liquid body, good consistency is arranged in the makeup organic phase, thereby can give full play to its performance.Add to them in makeup or as foodstuff additive, can bring into play the natural anticorrosion effect, also can be used as activeconstituents, alternative or reduce the consumption of Chemical Preservative, thereby further cater to people to the demand of makeup, the better security of food, have higher economic worth and wide market outlook.
Described prominent holder wax plum essential oil is as the purposes of antibacterial, anticorrosion, the antioxidant addn of preparation makeup and articles for washing.
Described prominent holder wax plum essential oil is as the purposes of preparation foodstuff additive.
Described prominent holder wax plum essential oil is as the purposes of preparation healthcare products.
The present invention adopts chromatography of gases-mass spectrometric hyphenated technique to be:
GC conditions: HP-5MS quartz capillary column (0.25mm*30m*0.25um), press 8.12psi before carrier gas 99.9995%He, post, 60 ℃ of column temperatures, after reservation 2min, 4 ℃/min is raised to 280 ℃, keeps 20min, the sample introduction temperature is 280 ℃, sample size 0.2 μ l, splitting ratio 50: 1;
The mass spectrum condition: ion source is EI, electron energy 70eV, 180 ℃ of ion source temperatures, 22 ℃ of transmission line temperature, sweep limit 50-550amu, solvent delay 3min;
Data processing and mass spectrum retrieval: sample air inlet phase Spectrometry, each separated portion adopt Nbs, Nist, Wiley to compose the storehouse retrieval-by-unification, and reference is confirmed, quantitatively adopts the chromatographic peak area normalization method.
Below in conjunction with the biological activity assay of prominent holder wax plum essential oil, further verify biological activity of the present invention and effect thereof.
(1) prominent holder wax plum essential oil sample of the present invention is to gram-positive microorganism (intestinal bacteria, Pseudomonas aeruginosa, Corynebacterium diphtheriae, dysentery bacterium); Antibacterial activity in vitro experimental technique and the result of Gram-negative bacteria (streptococcus aureus, subtilis, Sarcina lutea, bacillus thuringiensis, gas bacillus):
Testing method: with filter paper method test fungistatic effect; Pass through again minimum inhibitory concentration (MIC) and the minimal bactericidal concentration (MBC) of this volatile oil of constant broth dilution method determination.Substratum is respectively beef-protein medium and broth culture.
Show that by filter paper method bacteriostatic test certain density prominent holder wax plum essential oil sample all has obvious bacteriostatic action to this ten strains bacterium.Minimum inhibitory concentration MIC and minimum bactericidal concentration MBC are between 2-16mg/ml.Experiment shows that prominent holder wax plum essential oil tool is all inhibited to Gram-positive and negative bacterium, and the broad-spectrum antibacterial effect is arranged, and the results are shown in Table 1.
The prominent holder of table 1 wax plum essential oil is measured MIC and the MBC of tested bacterium:
(2) adopt reductibility, the test of DPPH free radical scavenging activity that the oxidation-resistance of prominent holder wax plum essential oil sample of the present invention is estimated:
Testing method:
Reductibility is measured: add sample liquid 1.0mL in test tube, phosphoric acid buffer (0.2M, pH6.6) 2.5mL, 1% Tripotassium iron hexacyanide 2.5mL.After 50 ℃ of water-bath 20min, add 10% trichoroacetic acid(TCA) 2.5mL, mixing is centrifugal.Get supernatant liquor 2.5mL and add distilled water 2.5mL and 0.1% iron trichloride 0.5mL.Measure absorbance after 10min at the 700nm place.The larger expression reducing power of absorbance is stronger.
The test of DPPH free radical scavenging activity: accurately take 10mgDPPH solution and dehydrated alcohol, and be settled to 250mL, DPPH concentration is 0.1mmol/L, keeps in Dark Place.With 2mL, 5mg/mL sample and 2mL DPPH solution add in same test tube, shake up, and measure its absorbancy with solvent as reference after placing 30min, measure simultaneously absorbancy after DPPH solution and solvent and the absorbancy after sample and solvent.Calculate according to the following formula clearance rate, the larger resistance of oxidation of clearance rate is stronger.(Vc) makes positive control with xitix.
DPPH clearance rate %=[1-(At-Ab)]/Ac*100
In formula: At is the absorbancy of sample and DPPH solution;
Ac is the absorbancy after DPPH solution and solvent;
Ab is the absorbancy after sample and solvent.
The anti-oxidant activity detection display, this essential oil has stronger reductibility, free radical scavenging activity its results are shown in Table 2 with table 3, IC 50=12.145mg/ml.
The prominent holder of table 2 wax plum reductibility is measured
Figure BSA00000349347800041
The prominent holder of table 3 wax plum essential oil DPPH free radical scavenging activity is measured
Figure BSA00000349347800042
(3) inhibitor effectiveness of the Microbial Challenge experimental test essential oil of employing makeup to makeup:
Testing method: with reference to the method for U.S.'s makeup, toilet articles and essence association (CTFA)
Tested bacterium: intestinal bacteria (Escherichia coil), streptococcus aureus (Staphylococcus aureus), Pseudomonas aeruginosa (Pseudomonas aeruginosa).
Experimental result indicates that tested bacteria concentration obviously reduces in 28 days, and this has further confirmed bacteriostatic activity and its validity as the makeup anticorrosive additive of this essential oil, and it the results are shown in Figure 2.
Useful achievement of the present invention:
(1) reported first of the present invention is extracted plants essential oil from prominent holder wax plum, and this essential oil has broad-spectrum antibacterial effect and good anti-oxidant activity.This aboundresources is the domestic endemic species in Jiangxi, distributes to concentrate, and is beneficial to exploitation, and preparation technology is reasonable, feasible, is easy to realize industrialization;
(2) plants essential oil provided by the invention can be applied in the industries such as cosmetics additive, foodstuff additive, medicinal and healthcare products.
Description of drawings
The growth-inhibiting figure [contain 5% prominent holder wax plum essential oil () and do not contain prominent holder wax plum essential oil (zero)] that Fig. 1 is intestinal bacteria of the present invention (Escherichia coil), streptococcus aureus (Staphylococcus aureus), Pseudomonas aeruginosa (Pseudomonas aeruginosa) in containing prominent holder wax plum essential oil and not adding the cosmetic base of essential oil.
Embodiment
Embodiment 1
(1) select the complete disease-free fresh blade of prominent holder wax plum, remove impurity, with flushing with clean water 3 times, natural air drying 24 hours, pulverize and sieve 20 orders, sealing saves backup;
(2) take the prominent holder of 30g wax plum powder in the 500ml flask, add 250ml distilled water, wet distillation 8 hours;
(3) distillate is loaded in separating funnel, standing 0.5 hour, reclaims the faint yellow transparent oily liquid in upper strata;
(4) remove moisture with anhydrous sodium sulfate drying, be prominent holder wax plum essential oil, in brown air-tight bottle-20 ℃ preservation.
The prominent holder wax plum essential oil that obtains is as the purposes of antibacterial, anticorrosion, the antioxidant addn of preparation makeup and articles for washing or as the purposes of foodstuff additive or as the purposes of healthcare products etc.
Embodiment 2
(1) select the complete disease-free fresh blade of prominent holder wax plum, remove impurity, with flushing with clean water 2 times, natural air drying 48 hours, pulverize and sieve 40 orders, sealing saves backup;
(2) take the prominent holder of 80g wax plum powder in the 1000ml round-bottomed flask, add water 500ml distilled water, wet distillation 7 hours;
(3) distillate is loaded in separating funnel, standing 0.5 hour, reclaims the faint yellow transparent oily liquid in upper strata;
(4) remove moisture with anhydrous sodium sulfate drying, be prominent holder wax plum essential oil, in brown air-tight bottle-20 ℃ preservation.
The prominent holder wax plum essential oil that obtains is as the purposes of antibacterial, anticorrosion, the antioxidant addn of preparation makeup and articles for washing or as the purposes of foodstuff additive or as the purposes of healthcare products etc.
Embodiment 3
(1) select the complete disease-free fresh blade of prominent holder wax plum, remove impurity, with flushing with clean water 3 times, natural air drying 36 hours, pulverize and sieve 60 orders, sealing saves backup;
(2) take the prominent holder of 50g wax plum powder in the 500ml flask, add 250ml distilled water, wet distillation 6 hours;
(3) distillate is loaded in separating funnel, standing 0.5 hour, reclaims the faint yellow transparent oily liquid in upper strata;
(4) remove moisture with anhydrous sodium sulfate drying, be prominent holder wax plum essential oil, in brown air-tight bottle-20 ℃ preservation.
The prominent holder wax plum essential oil that obtains is as the purposes of antibacterial, anticorrosion, the antioxidant addn of preparation makeup and articles for washing or as the purposes of foodstuff additive or as the purposes of healthcare products etc.

Claims (3)

1. prominent holder wax plum essential oil that utilizes extraction by steam distillation, it is characterized in that selecting prominent holder in autumn wax plum without the complete fresh leaf of scab, gather, clean, natural air drying, pulverize, distillation, oily water separation can obtain prominent holder wax plum essential oil, oil yield is 0.7-1.5%, its main chemical compositions is (E)-3-(4, 8-dimethyl-3, 7-nonene base)-furans 13.81%, acetyl norbornene ester 12.66%, 6, 6-dimethyl-3-methylene radical-dicyclo [3.1.1] heptane 7.06%, tetrahydrochysene solasodine 5.93%, loudspeaker enol 5.32%, 1, 5-dimethyl-1-vinyl-4 butyric acid hexene ester 5.09%, account for 49.87% of total volatile oil composition, this essential oil has purposes widely at cosmetic industry.
2. the preparation method of prominent holder wax plum essential oil according to claim 1 is characterized in that following these steps to carrying out:
(1) select the complete disease-free fresh blade of prominent holder wax plum in autumn, remove impurity, with flushing with clean water 1-3 time, natural air drying 12-48 hour, pulverize and sieve the 20-60 order, sealing saves backup;
(2) take a certain amount of prominent holder wax plum powder in round-bottomed flask, add water 5-10 and doubly measure, wet distillation 6-8 hour;
(3) distillate is loaded in separating funnel, standing 0.5 hour, reclaims the faint yellow transparent oily liquid in upper strata;
(4) remove moisture with anhydrous sodium sulfate drying, be prominent holder wax plum essential oil, yield is: 0.7%-1.5%, and in brown air-tight bottle-20 ℃ preservation.
3. prominent holder wax plum essential oil according to claim 1 is at preparation makeup and articles for washing is antibacterial, anticorrosion, the purposes of antioxidant addn.
CN2010105479090A 2010-11-17 2010-11-17 Medicinal and edible plant chimonanthus grammatus essential oil, and preparation method and application thereof Expired - Fee Related CN102002439B (en)

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CN104031744A (en) * 2014-06-27 2014-09-10 湖北五柳源生物科技有限责任公司 Supercritical CO2 extraction method for chimonanthus praecox essential oil
CN106244325A (en) * 2016-08-16 2016-12-21 重庆雅香美源生态农业科技有限公司 The extraction of a kind of Herba Acroptili repentis quintessence oil and processing method

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Publication number Priority date Publication date Assignee Title
CN1557411A (en) * 2004-01-17 2004-12-29 江西天海药业股份有限公司 Soft capsule of wintersweet leaf and its preparing method
CN101254221A (en) * 2007-07-20 2008-09-03 肖军平 Preparation of Chimonanthus nitens Oliv. oral liquid for preventing and controlling cold

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1557411A (en) * 2004-01-17 2004-12-29 江西天海药业股份有限公司 Soft capsule of wintersweet leaf and its preparing method
CN101254221A (en) * 2007-07-20 2008-09-03 肖军平 Preparation of Chimonanthus nitens Oliv. oral liquid for preventing and controlling cold

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