WO2021184633A1 - 具有防腐抑菌功能的复合植物提取物及其制备方法和应用 - Google Patents

具有防腐抑菌功能的复合植物提取物及其制备方法和应用 Download PDF

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WO2021184633A1
WO2021184633A1 PCT/CN2020/105120 CN2020105120W WO2021184633A1 WO 2021184633 A1 WO2021184633 A1 WO 2021184633A1 CN 2020105120 W CN2020105120 W CN 2020105120W WO 2021184633 A1 WO2021184633 A1 WO 2021184633A1
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extract
composite plant
plant extract
lemon
clove
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PCT/CN2020/105120
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English (en)
French (fr)
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巫世贵
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珠海市自然之旅生物技术有限公司
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08—Magnoliopsida [dicotyledons]
    • A01N65/36—Rutaceae [Rue family], e.g. lime, orange, lemon, corktree or pricklyash
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08—Magnoliopsida [dicotyledons]
    • A01N65/24—Lauraceae [Laurel family], e.g. laurel, avocado, sassafras, cinnamon or camphor
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08—Magnoliopsida [dicotyledons]
    • A01N65/28—Myrtaceae [Myrtle family], e.g. teatree or clove
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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]
    • A61K8/9789—Magnoliopsida [dicotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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]
    • A61K8/9794—Liliopsida [monocotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • 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
    • A61Q17/005—Antimicrobial preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/08—Anti-ageing preparations
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52—Stabilizers
    • A61K2800/524—Preservatives

Definitions

  • the invention belongs to the field of antiseptic technology, and particularly relates to a composite plant extract with antiseptic and antibacterial functions, and a preparation method and application thereof.
  • bacteriostatic preservatives that can be used in food and daily chemical products (such as cosmetics) in the prior art, such as a bacteriostatic and antiseptic composition composed of plant extracts such as peony grass, tea, thyme, sage, etc.
  • a bacteriostatic composition composed of plant extracts such as scutellaria root, panax notoginseng root, black soybean bark, honeysuckle flower, and plant extracts of wintergreen leaves, leeks, mint leaves, monkey earrings, sophora flavescens, etc. It is composed of bacteriostatic agent, but its addition amount in food or cosmetics is very high (mass fraction is 0.5% or more). Since the cost of plant extracts is higher than that of chemically synthesized or biosynthetic preservatives, coupled with the large amount of use, the cost of use will be high, which will undoubtedly reduce the customer's willingness to buy.
  • the present invention aims to solve at least one of the technical problems existing in the above-mentioned prior art.
  • the present invention proposes a composite plant extract with antiseptic and bacteriostatic functions.
  • the composite plant extract has a broad-spectrum bacteriostatic effect, and the addition amount in food and daily chemicals (such as cosmetics) is 0.04- 0.15% (mass fraction), the addition amount is small, and it also has a good antibacterial and antiseptic effect, which greatly reduces the use cost.
  • a composite plant extract with antiseptic and antibacterial functions comprising the following components: cinnamon extract, clove extract, lemon extract.
  • a compound plant extract with antiseptic and antibacterial functions in parts by weight, includes the following components: 3.5-50 parts of cinnamon extract, 3.5-92 parts of clove extract, and 1-20 parts of lemon extract .
  • the cinnamon extract is an extract of cinnamon bark.
  • the cinnamon extract contains trans-cinnamaldehyde and/or trans-o-methoxycinnamaldehyde.
  • the clove extract is a clove flower extract; further preferably, the clove extract is a clove bud extract and/or a clove leaf extract.
  • the clove extract contains isoeugenol and/or eugenol.
  • the lemon extract is lemon peel extract.
  • the lemon extract contains limonene.
  • the compound plant extract with antiseptic and antibacterial functions also includes turmeric extract.
  • the turmeric extract contains curcumin and/or gingerene.
  • the compound plant extract with antiseptic and antibacterial functions also includes orange peel extract.
  • the orange peel extract contains ⁇ -pinene.
  • the compound plant extract with antiseptic and antibacterial functions also includes star anise extract.
  • the star anise extract contains anisaldehyde.
  • the compound plant extract with antiseptic and antibacterial functions also contains limonene, bambooene, patchoule alcohol, baicalin, tanshinone, catechin, magnolol, carvacrol, thymol, myrcene, At least one of ⁇ -pin terpenes or carnosic acid.
  • the compound plant extract contains 3-40 parts of trans-cinnamaldehyde and 3-40 parts of trans-cinnamaldehyde in parts by weight of the active ingredients (active ingredients refer to the ingredients with antiseptic and bacteriostatic effects in each plant extract).
  • active ingredients refer to the ingredients with antiseptic and bacteriostatic effects in each plant extract.
  • the active ingredients of the composite plant extract in parts by weight, comprise 3-40 parts of trans-cinnamaldehyde, 0.1-5 parts of trans-o-methoxycinnamaldehyde, and 3-90 parts of isoeugenol.
  • eugenol 0.1-40 parts limonene 0.1-10 parts, limonene 0.1-10 parts, gingerene 0.05-5 parts, ⁇ -pinene 0.5-5 parts, curcumin 0.5-10 parts, anisaldehyde 0.5- 20 servings.
  • a preparation method of a compound plant extract with antiseptic and antibacterial functions includes the following steps:
  • cinnamon extract take cinnamon bark, add water, heat, steam to reflux, collect the reflux, then distill, collect the distillate, add organic solvent for extraction, and then heat to remove the organic solvent to prepare cinnamon extract Thing
  • the cinnamon bark in step (1) is powdered.
  • the organic solvent in step (1) is ether; further preferably, the organic solvent is ether.
  • the cloves in step (2) are clove buds and/or cloves leaves.
  • the organic solvent in step (2) is an ester; further preferably, the organic solvent is ethyl acetate.
  • rectification is performed at 103° C. to remove impurities.
  • the turmeric extract is also added during the stirring process in step (3), and the preparation method of the turmeric extract is: adding water to the turmeric, distilling, collecting the distillate, and fractionating under reduced pressure to prepare the turmeric extract.
  • the orange peel extract is also added during the stirring process in step (3), and the preparation method of the orange peel extract is: taking the orange peel, adding water, distilling, and collecting the distillate to prepare the orange peel extract.
  • the star anise extract is also added during the stirring process in step (3).
  • the preparation method of the star anise extract is as follows: add water to the star anise, distill, collect the distillate, and fractionate under reduced pressure to obtain the star anise extract Things.
  • step (3) limonene, bambooene, patchouli alcohol, baicalin, tanshinone, catechin, magnolol, carvacrol, thymol, myrcene, ⁇ -pin terpenes or At least one of carnosic acid.
  • step (3) at least one of turmeric extract, orange peel extract, star anise extract, limonene, bambooene, patchouli alcohol, baicalin, tanshinone, catechin or magnolol is added A sort of.
  • a daily chemical product containing the compound plant extract of the present invention is a daily chemical product containing the compound plant extract of the present invention.
  • the daily chemicals are cosmetics or bactericides.
  • the cosmetic is any one of moisturizing essence, eye cream, facial cleanser, and facial mask.
  • a food containing the compound plant extract of the present invention is a food containing the compound plant extract of the present invention.
  • the food is cooked food, such as kelp shreds and mustard tuber.
  • the content of the compound plant extract of the present invention in the cosmetic or food is 0.04-0.15% by mass fraction.
  • the compound plant extract of the present invention contains cinnamon extract, clove extract and lemon extract at the same time, and has a broad-spectrum antibacterial effect.
  • Candida albicans, Aspergillus niger, and Bacillus cereus have good bactericidal or inhibitory effects;
  • the added amount of the compound plant extract of the present invention in food and daily chemical products is 0.04-0.15% by mass fraction, and the added amount is small, and it also has a good antibacterial and antiseptic effect , Greatly reducing the cost of use.
  • the compound plant extract prepared by the present invention also has anti-oxidant effects.
  • the extraction method of the plant of the present invention has high extraction efficiency, and the prepared plant extract has a high content of active ingredients, for example, the extracted lemon extract has a high content of effective constituent limonene.
  • the raw materials, reagents or devices used in the following examples can be obtained from conventional commercial channels, or can be obtained by existing known methods.
  • a preparation method of a compound plant extract with antiseptic and antibacterial functions includes the following steps:
  • a preparation method of a compound plant extract with antiseptic and antibacterial functions includes the following steps:
  • the preparation method of the turmeric extract is: take 50Kg of turmeric powder and add 200L of water, distill to obtain 20L of distillate, and remove impurities by fractional distillation under reduced pressure Refined to obtain 19Kg of turmeric extract, stirring, stirring at a speed of 60 rpm, stirring time of 30 minutes, to prepare a composite plant extract; the prepared composite plant extract is 200Kg, of which trans-cinnamaldehyde is 12.5Kg , Trans o-methoxycinnamaldehyde 2.5Kg, isoeugenol 120Kg, limonene 3Kg, curcumin 7.6Kg, gingerene 1.9Kg.
  • a preparation method of a compound plant extract with antiseptic and antibacterial functions includes the following steps:
  • the preparation method of turmeric extract is: take 20Kg of turmeric powder and add 200L of water, distill to obtain 20L of distillate, and purify by vacuum fractional distillation to remove impurities to obtain 7.6Kg of plant extract containing curcumin and gingerene;
  • the preparation method of orange peel extract is: take 30Kg of orange peel, add 180L of water, distill, collect 15L of distillate, prepare 6Kg of orange peel extract containing ⁇ -pinene;
  • the preparation method of star anise extract is: take 40Kg star anise, add 200L of water, steam distillation extraction, repeat the extraction twice to collect a total of 30L of distillate, and fractionate under reduced pressure to obtain 5.4Kg of star anise extract containing anisaldehyde;
  • the stirring speed is 60 rpm, and the stirring time is 30 minutes to prepare a composite plant extract;
  • the prepared composite plant extract is 200Kg, of which the trans-cinnamaldehyde is 12.5Kg, and the trans-o-methoxycinnamaldehyde is 12.5Kg.
  • 2.5Kg isoeugenol 120Kg, limonene 3Kg, curcumin 3Kg, gingerene 1.3Kg, ⁇ -pinene 3Kg, and anisaldehyde 4Kg.
  • a preparation method of a compound plant extract with antiseptic and antibacterial functions includes the following steps:
  • a composite plant extract is obtained; the prepared composite plant extract is 200Kg, of which trans-cinnamaldehyde is 15Kg, trans-o-methoxycinnamaldehyde is 3Kg, isoeugenol is 120Kg, limonene is 5Kg, bambooene is 1Kg, and patchouli alcohol 0.3Kg.
  • the composite plant extracts prepared in Examples 1-3 of the present invention are effective against Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, Candida albicans, Aspergillus niger, and Bacillus cereus.
  • the minimum inhibitory concentrations of Bacillus subtilis and Bacillus subtilis are significantly lower than the minimum inhibitory concentrations of sodium dehydroacetate, potassium sorbate and sodium benzoate, indicating that the compound plant extracts prepared in Examples 1-3 of the present invention have good antibacterial effects .
  • Table 3 shows the toxicity levels of the composite plant extract and common antibacterial preservatives prepared in Example 2 of the present invention.
  • the composite plant extract prepared in Example 2 of the present invention is a non-toxic substance, which is more safe when added to food.
  • Example 3 Take the compound plant extract prepared in Example 3, two common plant preservatives A and B on the market (preservative A mainly contains Paeonia Suffruticosa extract and Qinjiao extract, and Preservative B mainly contains Zhimu extract , Magnolia Bark Extract), sensory evaluation was conducted to evaluate the sensory scores on smell and taste (taste). The maximum score is 5. The higher the score, the higher the acceptance and the stronger the sense of pleasure. The results are shown in Table 4. .
  • Example 3 of the present invention has a higher score than the two common plant preservatives A and B that are commercially available. It can be seen that the composite plant extract prepared in Example 3 of the present invention has a higher score. The compound plant extracts have better sensory evaluation.
  • Example 5 Moisturizing essence containing the compound plant extract prepared by the present invention
  • the antiseptic challenge method is to add a certain amount of microorganisms to the moisturizing essence to simulate the possible contamination in the cosmetics, and to test the amount of viable bacteria at regular intervals to judge the effectiveness of the cosmetic antiseptic system based on the increase or decrease of viable bacteria Experimental method.
  • the anti-corrosion challenge test evaluation standard is the standard in Table 7 below, and meeting this standard can be judged as passing the anti-corrosion challenge test.
  • the moisturizing essence contains the compound plant extract prepared in Example 1 and Example 4 at a concentration of 0.06% to pass the preservative challenge.
  • the moisturizing essence contains benzene.
  • the oxyethanol needs to be added to 0.8% to pass the anti-corrosion challenge.
  • Example 2 and Example 3 of the present invention were added to cooked kelp shreds, and the total number of colonies data during shelf life was tracked (the tracking results are shown in Table 10) to verify the composite extract prepared by the present invention Antibacterial ability in food.
  • Kelp shreds blanching the soaking water shall be based on submerging the kelp shreds, soak for 5 minutes at 85°C;
  • Table 10 Tracking results of the total number of colonies in the shelf life of kelp silk (log cfu/g)

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Abstract

本发明属于防腐技术领域，公开了一种具有防腐抑菌功能的复合植物提取物，包括以下组分：肉桂提取物、丁香提取物、柠檬提取物。所述柠檬提取物中含有苧烯；该复合植物提取物还可包括姜黄提取物、橘皮提取物或八角茴香提取物中的至少一种。该复合植物提取物同时包含肉桂提取物、丁香提取物和柠檬提取物，具有广谱抑菌效果，对金黄色葡萄球菌、大肠埃希氏菌、铜绿假单胞菌、白色念珠菌、黑曲霉、蜡样芽孢杆菌具有很好的杀菌或抑制效果；该复合植物提取物在食品和日化用品中的添加量，按质量分数计，为0.04-0.15％，添加量少，还具有很好的抑菌防腐效果，大大降低使用成本。

Description

具有防腐抑菌功能的复合植物提取物及其制备方法和应用 技术领域
本发明属于防腐技术领域，特别涉及一种具有防腐抑菌功能的复合植物提取物及其制备方法和应用。
背景技术
现有技术中，常见的防腐剂大多是化学合成和生物合成的，其具有一定的慢性毒副作用且应用限制较多，并且多存在只对某一种或几种菌有抑制作用，要得到广谱抑菌的效果就要复配多种防腐剂。
现有技术中也有可用于食品和日化产品(例如化妆品)中的天然植物抑菌防腐剂，如一种由透骨草、茶叶、百里香、鼠尾草等植物提取物组成的抑菌防腐组合物，一种由黄芩根、三七根、黑豆皮、忍冬花等植物提取物组成的具有抑菌功效的组合物，还有由冬青叶、韭菜、薄荷叶、猴耳环、苦参等植物提取物组成的抑菌剂，但其在食品或化妆品中的添加量都很高(质量分数为0.5％以上的添加量)。由于植物提取物成本本身就较化学合成或生物合成的防腐剂要高，再加上使用量大，使用成本就会很高，无疑会降低客户购买意愿。
因此，希望提供一种具有广谱抑菌效果，且在食品或日化用品(例如化妆品)中添加量少的植物提取物。
发明内容
本发明旨在至少解决上述现有技术中存在的技术问题之一。为此，本发明提出一种具有防腐抑菌功能的复合植物提取物，所述复合植物提取物具有广谱抑菌效果，且在食品和日化用品(例如化妆品)中的添加量为0.04-0.15％(质量分数)，添加量少，还具有很好的抑菌防腐效果，大大降低使用成本。
一种具有防腐抑菌功能的复合植物提取物，包括以下组分：肉桂提取物、丁香提取物、柠檬提取物。
优选的，一种具有防腐抑菌功能的复合植物提取物，按重量份数计，包括以下组分：肉桂提取物3.5-50份、丁香提取物3.5-92份、柠檬提取物1-20份。
优选的，所述肉桂提取物为肉桂树皮提取物。
优选的，所述肉桂提取物中包含反式肉桂醛和/或反式邻甲氧基肉桂醛。
优选的，所述丁香提取物为丁香花提取物；进一步优选的，所述丁香提取物为丁香花蕾提取物和/或丁香叶提取物。
优选的，所述丁香提取物中包含异丁香酚和/或丁香酚。
优选的，所述柠檬提取物为柠檬皮提取物。
优选的，所述柠檬提取物中含有苧烯。
优选的，所述具有防腐抑菌功能的复合植物提取物还包括姜黄提取物。所述姜黄提取物中含有姜黄素和/或姜烯。
优选的，所述具有防腐抑菌功能的复合植物提取物还包括橘皮提取物。所述橘皮提取物中含有α-蒎烯。
优选的，所述具有防腐抑菌功能的复合植物提取物还包括八角茴香提取物。所述八角茴香提取物中含有大茴香醛。
优选的，所述具有防腐抑菌功能的复合植物提取物中还含有柠檬烯、竹烯、广藿香醇、黄芩苷、丹参酮、儿茶素、厚朴酚、香芹酚、百里香酚、月桂烯、β-蒎萜类或鼠尾草酸中的至少一种。
优选的，所述复合植物提取物，其有效成分(有效成分是指各植物提取物中有防腐抑菌效果的成分)，按重量份数计，包含反式肉桂醛3-40份、反式邻甲氧基肉桂醛0.1-5份、异丁香酚3-90份、苧烯0.1-10份。
进一步优选的，所述复合植物提取物，其有效成分，按重量份数计，包含反式肉桂醛3-40份、反式邻甲氧基肉桂醛0.1-5份、异丁香酚3-90份、丁香酚0.1-40份、苧烯0.1-10份、柠檬烯0.1-10份、姜烯0.05-5份、α-蒎烯0.5-5份、姜黄素0.5-10份、大茴香醛0.5-20份。
一种具有防腐抑菌功能的复合植物提取物的制备方法，包括以下步骤：
(1)肉桂提取物的制备：取肉桂树皮，加水，加热，蒸汽冷凝回流，收集回流液，再进行蒸馏，收集馏出液，加有机溶剂萃取，再加热去除有机溶剂，制得肉桂提取物；
(2)丁香提取物的制备：取丁香，加水，蒸馏，收集馏出液，加有机溶剂萃取，减压分馏，除去有机溶剂，制得丁香提取物；
(3)柠檬提取物的制备：取柠檬，用冷压榨法(冷压榨法是本行业常规技术)或蒸馏法制得柠檬提取物；然后加入步骤(1)制得的肉桂提取物和步骤(2)制得的丁香提取物，搅拌，制得所述复合植物提取物。
优选的，步骤(1)中所述肉桂树皮为粉末状。
优选的，步骤(1)中所述有机溶剂为醚；进一步优选的，所述有机溶剂为***。
优选的，步骤(2)中所述丁香为丁香花蕾和/或丁香叶。
优选的，步骤(2)中所述有机溶剂为酯；进一步优选的，所述有机溶剂为乙酸乙酯。
优选的，步骤(3)中经过冷压榨法提取柠檬后，在103℃下进行精馏，除杂。
优选的，步骤(3)中搅拌过程中还加入姜黄提取物，所述姜黄提取物的制备方法为：取姜黄加水，蒸馏，收集馏出液，减压分馏，制得姜黄提取物。
优选的，步骤(3)中搅拌过程中还加入橘皮提取物，所述橘皮提取物的制备方法为：取橘皮，加水，蒸馏，收集馏出液，制得橘皮提取物。
优选的，步骤(3)中搅拌过程中还加入八角茴香提取物，所述八角茴香提取物的制备方法为：取八角茴香加水，蒸馏，收集馏出液，减压分馏，制得八角茴香提取物。
优选的，步骤(3)中搅拌过程还加入柠檬烯、竹烯、广藿香醇、黄芩苷、丹参酮、儿茶素、厚朴酚、香芹酚、百里香酚、月桂烯、β-蒎萜类或鼠尾草酸中的至少一种。
优选的，步骤(3)中搅拌过程还加入姜黄提取物、橘皮提取物、八角茴香提取物、柠檬烯、竹烯、广藿香醇、黄芩苷、丹参酮、儿茶素或厚朴酚中的至少一种。
一种日化用品，含有本发明所述的复合植物提取物。
优选的，所述日化用品为化妆品或杀菌剂。
优选的，所述化妆品为保湿精华液、眼霜、洗面奶、面膜中的任意一种。
一种食品，含有本发明所述的复合植物提取物。
优选的，所述食品为熟食，例如海带丝、榨菜。
优选的，所述化妆品或食品中，本发明所述复合植物提取物的含量，按质量分数计，为0.04-0.15％。
相对于现有技术，本发明的有益效果如下：
(1)本发明所述复合植物提取物同时包含肉桂提取物、丁香提取物和柠檬提取物，具有 广谱抑菌效果，对对金黄色葡萄球菌、大肠埃希氏菌、铜绿假单胞菌、白色念珠菌、黑曲霉、蜡样芽孢杆菌具有很好的杀菌或抑制效果；
(2)本发明所述复合植物提取物在食品和日化用品(例如化妆品)中的添加量，按质量分数计，为0.04-0.15％，添加量少，还具有很好的抑菌防腐效果，大大降低使用成本。另外，本发明制得的复合植物提取物还具有抗氧化的功效。
(3)本发明所述植物的提取方法提取效率高，制得的植物提取物中有效成分含量高，例如提取的柠檬提取物中有效组成苧烯的含量高。
具体实施方式
为了让本领域技术人员更加清楚明白本发明所述技术方案，现列举以下实施例进行说明。需要指出的是，以下实施例对本发明要求的保护范围不构成限制作用。
以下实施例中所用的原料、试剂或装置如无特殊说明，均可从常规商业途径得到，或者可以通过现有已知方法得到。
实施例1
一种具有防腐抑菌功能的复合植物提取物的制备方法，包括以下步骤：
(1)肉桂提取物的制备：取60Kg粉状的肉桂树皮，放入烧瓶中，加水160L，加热至100℃，蒸汽冷凝回流10分钟，收集回流液，冷却，再进行蒸馏，收集馏出液90L，将馏出液转移至分液漏斗中，加***萃取2次，***每次的用量为40L，弃去水层，将***层移入试管中，加入少量无水硫酸钠干燥，20分钟后，倒出萃取液，在通风橱内用水浴加热蒸去***，制得含反式肉桂醛和反式邻甲氧基肉桂醛的肉桂提取物30Kg；
(2)丁香提取物的制备：取丁香花蕾500Kg，加水3000L，蒸馏，收集馏出液1000L，将所得的馏出液置于分液漏斗中，用乙酸乙酯萃取两次(每次乙酸乙酯的用量为600L)，合并上层乙酸乙酯萃取液，之后进行减压分馏将乙酸乙酯去除，制得含异丁香酚的丁香提取物150Kg；
(3)柠檬提取物的制备：取100Kg柠檬皮，用冷压榨法处理柠檬皮，除杂，制得含苧烯的柠檬提取物20Kg；然后加入步骤(1)制得的肉桂提取物和步骤(2)制得的丁香提取物，搅拌，搅拌速度为60转/分钟，搅拌时间为30分钟，制得复合植物提取物；制得的复合植物提取物为200Kg，其中反式肉桂醛为15Kg，反式邻甲氧基肉桂醛3Kg，异丁香酚120Kg，苧 烯10Kg。
实施例2
一种具有防腐抑菌功能的复合植物提取物的制备方法，包括以下步骤：
(1)肉桂提取物的制备：取50Kg粉状的肉桂树皮，放入烧瓶中，加水160L，加热至100℃，蒸汽冷凝回流10分钟，收集回流液，冷却，再进行蒸馏，收集馏出液80L，将馏出液转移至分液漏斗中，加***萃取2次，***每次的用量为40L，弃去水层，将***层移入试管中，加入少量无水硫酸钠干燥，20分钟后，倒出萃取液，在通风橱内用水浴加热蒸去***，制得含反式肉桂醛和反式邻甲氧基肉桂醛的肉桂提取物25Kg；
(2)丁香提取物的制备：取丁香花叶500Kg，加水3000L，蒸馏，收集馏出液1000L，将所得的馏出液置于分液漏斗中，用乙酸乙酯萃取两次(每次乙酸乙酯的用量为600L)，合并上层乙酸乙酯萃取液，之后进行减压分馏将乙酸乙酯去除，制得含异丁香酚的丁香提取物150Kg；
(3)柠檬提取物的制备：取30Kg柠檬皮，加水180L，蒸馏，获得馏出液10L，制得含苧烯的柠檬提取物6Kg；然后加入步骤(1)制得的肉桂提取物和步骤(2)制得的丁香提取物，再加入含姜黄素和姜烯的姜黄提取物，姜黄提取物的制备方法为：取50Kg姜黄粉末加水200L，蒸馏获得馏出液20L，减压分馏除杂精制，制得姜黄提取物19Kg，搅拌，搅拌速度为60转/分钟，搅拌时间为30分钟，制得复合植物提取物；制得的复合植物提取物为200Kg，其中反式肉桂醛为12.5Kg，反式邻甲氧基肉桂醛2.5Kg，异丁香酚120Kg，苧烯3Kg，姜黄素7.6Kg、姜烯1.9Kg。
实施例3
一种具有防腐抑菌功能的复合植物提取物的制备方法，包括以下步骤：
(1)肉桂提取物的制备：取50Kg粉状的肉桂树皮，放入烧瓶中，加水160L，加热至100℃，蒸汽冷凝回流10分钟，收集回流液，冷却，再进行蒸馏，收集馏出液85L，将馏出液转移至分液漏斗中，加***萃取2次，***每次的用量为40L，弃去水层，将***层移入试管中，加入少量无水硫酸钠干燥，20分钟后，倒出萃取液，在通风橱内用水浴加热蒸去***，制得含反式肉桂醛和反式邻甲氧基肉桂醛的肉桂提取物25Kg；
(2)丁香提取物的制备：取丁香花蕾500Kg，加水3000L，蒸馏，收集馏出液1000L， 将所得的馏出液置于分液漏斗中，用乙酸乙酯萃取两次(每次乙酸乙酯的用量为600L)，合并上层乙酸乙酯萃取液，之后进行减压分馏将乙酸乙酯去除，制得含异丁香酚的丁香提取物150Kg；
(3)柠檬提取物的制备：取30Kg柠檬皮，加水180L，蒸馏，获得馏出液10L，制得含苧烯的柠檬提取物6Kg；然后加入步骤(1)制得的肉桂提取物和步骤(2)制得的丁香提取物，再加入姜黄提取物、橘皮提取物和八角茴香提取物；
姜黄提取物的制备方法为：取20Kg姜黄粉末加水200L，蒸馏获得馏出液20L，减压分馏除杂精制，制得含姜黄素和姜烯的植物提取物7.6Kg；
橘皮提取物的制备方法为：取30Kg橘皮，加水180L，蒸馏，收集馏出液15L，制得含α-蒎烯的橘皮提取物6Kg；
八角茴香提取物的制备方法为：取40Kg八角茴香加水200L，水蒸气蒸馏提取，重复提取2次收集馏出液共30L，减压分馏，制得含大茴香醛的八角茴香提取物5.4Kg；
搅拌，搅拌速度为60转/分钟，搅拌时间为30分钟，制得复合植物提取物；制得的复合植物提取物为200Kg，其中反式肉桂醛为12.5Kg，反式邻甲氧基肉桂醛2.5Kg，异丁香酚120Kg，苧烯3Kg，姜黄素3Kg、姜烯1.3Kg、α-蒎烯3Kg、大茴香醛4Kg。
实施例4
一种具有防腐抑菌功能的复合植物提取物的制备方法，包括以下步骤：
(1)肉桂提取物的制备：取60Kg粉状的肉桂树皮，放入烧瓶中，加水160L，加热至100℃，蒸汽冷凝回流10分钟，收集回流液，冷却，再进行蒸馏，收集馏出液90L，将馏出液转移至分液漏斗中，加***萃取2次，***每次的用量为40L，弃去水层，将***层移入试管中，加入少量无水硫酸钠干燥，20分钟后，倒出萃取液，在通风橱内用水浴加热蒸去***，制得含反式肉桂醛和反式邻甲氧基肉桂醛的肉桂提取物30Kg；
(2)丁香提取物的制备：取丁香花蕾500Kg，加水3000L，蒸馏，收集馏出液1000L，将所得的馏出液置于分液漏斗中，用乙酸乙酯萃取两次(每次乙酸乙酯的用量为600L)，合并上层乙酸乙酯萃取液，之后进行减压分馏将乙酸乙酯去除，制得含异丁香酚的丁香提取物150Kg；
(3)柠檬提取物的制备：取50Kg柠檬皮，用冷压榨法处理柠檬皮，除杂，制得含苧烯 的柠檬提取物10Kg；
(4)广藿香提取物的制备：取50Kg广藿香，加水400L，蒸馏，收集馏出液40L，减压蒸馏，得含竹烯和广藿香醇的广藿香提取物10Kg，然后加入步骤(1)制得的肉桂提取物、步骤(2)制得的丁香提取物和步骤(3)制得的檬提取物，搅拌，搅拌速度为60转/分钟，搅拌时间为30分钟，制得复合植物提取物；制得的复合植物提取物为200Kg，其中反式肉桂醛为15Kg，反式邻甲氧基肉桂醛3Kg，异丁香酚120Kg，苧烯5Kg，竹烯1Kg，广藿香醇0.3Kg。
产品效果测试
1.广谱抑菌测试
取实施例1-3制得的复合植物提取物、脱氢乙酸钠、山梨酸钾和苯甲酸钠(脱氢乙酸钠、山梨酸钾和苯甲酸钠为常规抑菌防腐剂)，测试其最小抑菌浓度(MIC，单位：ppm)，结果如表1所示。
表1：
Figure PCTCN2020105120-appb-000001
从表1可以看出，本发明实施例1-3制得的复合植物提取物对金黄色葡萄球菌、大肠埃希氏菌、铜绿假单胞菌、白色念珠菌、黑曲霉、蜡样芽孢杆菌和枯草芽孢杆菌的最小抑菌浓度明显低于脱氢乙酸钠、山梨酸钾和苯甲酸钠的最小抑菌浓度，表明本发明实施例1-3制得的复合植物提取物具有好的抑菌效果。
2.毒性测试
按照标准GB15193.3-2014，对物质进行急性大鼠口服毒性分级，如表2所示。本发明实施例2制得的复合植物提取物与常见抑菌防腐剂的毒性级别如表3所示。
表2：
级别 大鼠口服半数致死量(LD50)/(mg/Kg)
急毒 <1
剧毒 1-50
中等毒 51-500
低毒 501-5000
无毒 >5000
表3：
Figure PCTCN2020105120-appb-000002
从表2和表3可以看出，本发明实施例2制得的复合植物提取物属于无毒物质，添加到食品，安全性更高。
3.感官评价
取实施例3制得的复合植物提取物、市售的2种常见植物防腐剂A和防腐剂B(防腐剂A主要含牡丹皮提取物、秦椒提取物，防腐剂B主要含知母提取物、厚朴提取物)，进行感官评价，评价在气味和口感(滋味)上的感官分数，满分5分，分数越高，代表接受程度更高，愉悦感更强，结果如表4所示。
表4：
Figure PCTCN2020105120-appb-000003
Figure PCTCN2020105120-appb-000004
从表4可以看出，本发明实施例3制得的复合植物提取物相对于市售的2种常见植物防腐剂A和防腐剂B有更高的评分，可见，本发明实施例3制得的复合植物提取物有更好的感官评价。
4.抗氧化性测试
取实施例1-4制得的复合植物提取物和市售常见的抗氧化物质迷迭香提取物(主要成分为鼠尾草酸)、茶多酚、特丁基对苯二酚，测试抗氧化性能。抗氧化能力评价方法：在同样的浓度下(50ppm)下，测试自由基清除率(％)，清除率越高，代表抗氧化能力越强，结果如表5所示。
表5：
抗氧化剂(50ppm) 自由基清除率(％)
实施例1 20.76
实施例2 21.08
实施例3 20.55
实施例4 22.04
迷迭香提取物(鼠尾草酸) 7.85
茶多酚 58.20
特丁基对苯二酚 40.05
从表5可以看出，本发明实施例1-4制得的复合植物提取物具有一定的抗氧化性能。
实施例5：含本发明制得的复合植物提取物的保湿精华液
按4种配方，配成保湿精华液，分别为保湿精华液a、保湿精华液b、保湿精华液c和保湿精华液d，各组具体配方如表6所示。
表6：
Figure PCTCN2020105120-appb-000005
从表6可以看出，本发明制得的复合植物提取物添加到保湿精华液，并通过防腐挑战试验验证其防腐效果。防腐挑战方法即是将一定量的微生物加入到保湿精华液中，模拟化妆品 中可能出现的污染情况，每隔一定时间对其中的活菌量进行检测，以活菌增减量判断化妆品防腐体系效能的实验方法。
具体的步骤如下：
(1)将样品(即表6中对应的4种保湿精华液)在无菌环境下分装至灭菌小盒中，均分为两组，分别为细菌组和真菌组，在样品小盒中加入菌液后混匀，细菌组细菌浓度为7logcfu/g(例如10 7cfu/g＝7log cfu/g)，真菌组真菌浓度为4log cfu/g；
(2)分别称量样品5mL，分别放入含有45mL无菌稀释液中，混匀，制得10 -1(即样品的体积浓度为10％)样品匀液；
(3)吸取1mL 10 -1样品匀液，加入9mL灭菌稀释液，制成10 -2的样品匀液，按此方法进行10倍递增稀释至合适浓度(每递增稀释一次，换用1次1mL吸头)；
(4)吸取1mL样品匀液于无菌平皿内，将冷却至46℃的营养琼脂培养基和孟加拉虎红培养基倾注平皿，并转动平皿使其混合均匀；
(5)待平皿里琼脂完全凝固，做好标记，倒置平皿放入恒温培养箱，细菌于37℃培养24-48h，真菌于27℃培养5-7天；
(6)每7天检测一次，共5次28天。
评价标准
防腐挑战试验评价标准为下表7标准，满足该标准即可判定为通过防腐挑战测试。
表7：标准
Figure PCTCN2020105120-appb-000006
Figure PCTCN2020105120-appb-000007
防腐挑战结果如表8所示：
表8：
Figure PCTCN2020105120-appb-000008
从表8(ND表示未检测到)可以看出，保湿精华液中含有实施例1和实施例4制得的复合植物提取物的浓度为0.06％即可通过防腐挑战，保湿精华液中含苯氧乙醇的需要加到0.8％才能通过防腐挑战。
实施例6
在熟食海带丝中添加本发明实施例2和实施例3制得的复合植物提取物，通过货架期的菌落总数数据跟踪(追踪结果如表10所示)，验证本发明制得的复合提取物在食品中的抑菌能力。
四种海带丝的组分如表9所示。
表9：
Figure PCTCN2020105120-appb-000009
Figure PCTCN2020105120-appb-000010
海带丝的制作工艺为：
(1)海带丝热烫：浸泡水以淹没海带丝为准，85℃条件下浸泡5分钟；
(2)调味：热烫后捞出海带丝，沥水15分钟，依次加入食盐、白砂糖、味精、白米醋、鸡粉、香油、辣椒油，搅拌均匀后静置15分钟，以待海带丝入味(实施例2和实施例3制得的复合植物提取物在步骤(2)中加入)；
(3)包装：蒸煮袋真空包装，真空时间30秒，热封口时间2秒，冷却时间2秒；
(4)灭菌工艺：常压，恒温100℃，水浴20分钟。
表10：海带丝货架期菌落总数跟踪结果(log cfu/g)
Figure PCTCN2020105120-appb-000011
Figure PCTCN2020105120-appb-000012
从表10(大于或等于4.5为超标，ND表示未检测到)可以看出，添加了本发明实施例2和实施例3制得的复合植物提取物的海带丝在6周内可以保证微生物含量不超标，有较好的防腐效果。

Claims (10)

  1. 一种复合植物提取物，其特征在于，包括以下组分：肉桂提取物、丁香提取物、柠檬提取物。
  2. 根据权利要求1所述的复合植物提取物，其特征在于，所述柠檬提取物中含有苧烯。
  3. 根据权利要求1所述的复合植物提取物，其特征在于，所述复合植物提取物还包括姜黄提取物、橘皮提取物或八角茴香提取物中的至少一种。
  4. 根据权利要求1所述的复合植物提取物，其特征在于，所述复合植物提取物中还含有柠檬烯、竹烯、广藿香醇、黄芩苷、丹参酮、儿茶素、厚朴酚、香芹酚、百里香酚、月桂烯、β-蒎萜类或鼠尾草酸中的至少一种。
  5. 根据权利要求1所述的复合植物提取物，其特征在于，所述复合植物提取物，其有效成分，按重量份数计，包含反式肉桂醛3-40份、反式邻甲氧基肉桂醛0.1-5份、异丁香酚3-90份、苧烯0.1-10份。
  6. 权利要求1-5中任一项所述的复合植物提取物的制备方法，其特征在于，包括以下步骤：
    (1)肉桂提取物的制备：取肉桂树皮，加水，加热，蒸汽冷凝回流，收集回流液，再进行蒸馏，收集馏出液，加有机溶剂萃取，再加热去除有机溶剂，制得肉桂提取物；
    (2)丁香提取物的制备：取丁香，加水，蒸馏，收集馏出液，加有机溶剂萃取，减压分馏，除去有机溶剂，制得丁香提取物；
    (3)柠檬提取物的制备：取柠檬，用冷压榨法或蒸馏法制得柠檬提取物；然后加入步骤(1)制得的肉桂提取物和步骤(2)制得的丁香提取物，搅拌，制得所述复合植物提取物。
  7. 根据权利要求6所述的制备方法，其特征在于，步骤(3)中搅拌过程中还加入姜黄提取物、橘皮提取物、八角茴香提取物、柠檬烯、竹烯、广藿香醇、黄芩苷、丹参酮、儿茶素、厚朴酚、香芹酚、百里香酚、月桂烯、β-蒎萜类或鼠尾草酸中的至少一种。
  8. 一种日化用品，其特征在于，所述日化用品含有权利要求1-5中任一项所述的复合植物提取物。
  9. 一种食品，其特征在于，所述食品含有权利要求1-5中任一项所述的复合植物提取物。
  10. 根据权利要求9所述的食品，其特征在于，所述复合植物提取物的含量，按质量分数 计，为0.04-0.15％。
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