Summary of the invention
The object of this invention is to provide the application of a kind of Callicarpa nudiflora extract in daily use chemicals cleaning product.By Callicarpa nudiflora extract, add in handwashing liquid, soap, foot lotion, bath foam, liquid detergent series daily use chemicals cleaning product.
(1) preparation of Callicarpa nudiflora extract
Callicarpa nudiflora extract of the present invention is water, alcohol or the diluted ketone extraction thing of fresh or dry Callicarpa nudiflora raw material.
Callicarpa nudiflora extract of the present invention is prepared by following any method:
(1) adopt the fresh or dried feed of Callicarpa nudiflora, add water or rare alcohol or rare ketone solvent, heating extraction, extracting solution filters, and filtrate is concentrated, the dry Callicarpa nudiflora extract A that to obtain;
(2) adopt the fresh or dried feed of Callicarpa nudiflora, add water or rare alcohol or rare ketone solvent, heating extraction, extracting solution filters, and filtrate is passed through macroporous adsorbent resin column chromatography, wash cylinder with water, discard water lotion, then use 10%~90% ethanol elution, eluent filters, concentrated, be dried to obtain Callicarpa nudiflora extract B;
(3) the Callicarpa nudiflora raw material of fresh state, obtains pressed liquor and press residue through squeezing, and pressed liquor filters, and filtrate is concentrated, is dried to obtain Callicarpa nudiflora extract C;
(4) the Callicarpa nudiflora raw material of employing fresh state, obtains pressed liquor and press residue through squeezing, and press residue adds water or rare alcohol or rare ketone solvent, heating extraction, and extracting solution and pressed liquor merge, and filter, and filtrate is concentrated, is dried to obtain Callicarpa nudiflora extract D;
(5) the Callicarpa nudiflora raw material of employing fresh state, obtains pressed liquor and press residue through squeezing, and press residue adds water or rare alcohol or rare ketone solvent, heating extraction, extracting solution and pressed liquor merge, and filter, and filtrate is passed through macroporous adsorbent resin column chromatography, wash cylinder with water, discard water lotion, then use 10%~90% ethanol elution, eluent filters, concentrated, be dried to obtain Callicarpa nudiflora extract E;
(6) adopt fresh or dry Callicarpa nudiflora raw material, add water or rare alcohol or rare ketone decoction secondary, collecting decoction, filters, concentrated, carry out membrane filtration, first use ultrafiltration then nanofiltration, ceramic composite membrane and poly tetrafluoroethylene for membrane material, concentrated, be dried to obtain Callicarpa nudiflora F.
The raw material of Callicarpa nudiflora extract adopts the Callicarpa nudiflora aerial parts of fresh or drying regime, preferably fresh summer and Callicarpa nudiflora leaf and/or the twig in autumn.
Squeezing described in method (3) to (5) is that to adopt weight ratio be 1 ~ 3:1, and water or rare alcohol or rare ketone mix with fresh Callicarpa nudiflora.
Inventor farthest extracts effective active composition in order to realize from Callicarpa nudiflora, extracting mode (squeeze, heat), collecting time (spring, summer, autumn, winter) and the different drying regime (fresh, dry product) of inventor to Callicarpa nudiflora carried out systematic study, and result is as following table 1:
Table 1:
Attention: above index is all by fresh goods.
In conventional extraction process, the general Callicarpa nudiflora for drying used, extraction yield, total flavones and the luteolin of result of study explanation Callicarpa nudiflora, total tannin content and collecting season, extracting mode are relevant with medicinal material drying state.
1) extraction yield, total flavones and the luteolin of the Callicarpa nudiflora heating extraction of fresh state, total tannin content are all high than dry product mutually of the same period.The Callicarpa nudiflora of gathering taking autumn is as example, extraction yield in fresh Callicarpa nudiflora, general flavone content, luteolin, total tannin content are respectively 1.20,1.59,1.52,1.05 times of dry product, illustrate raw material effective ingredient in dry run forfeiture major part.
2), compared with heating extraction, squeeze the obvious yield that improves Callicarpa nudiflora, total flavones and luteolin, total tannin content.The Callicarpa nudiflora of gathering taking autumn is as example, and yield, general flavone content, the content of luteolin that fresh Callicarpa nudiflora squeezes is respectively 1.13,1.23,1.20,1.14 times of dry product.
3) yield of the Callicarpa nudiflora of different collecting seasons, total flavones and luteolin, total tannin content have different, and research shows that extraction yield, total flavones and the luteolin in summer and period in autumn, total tannin content are better than spring and winter.
(2) preparation of Callicarpa nudiflora series daily use chemicals cleaning product:
1, handwashing liquid
Prescription: (%) meter by weight, surfactant 10-55%(is as polyoxyethylenated alcohol sodium sulfate 3-20%, lauryl alcohol sulfuric ester triethanolamine salt 3-15%, dodecyldimethylammonium hydroxide inner salt 3-15%, lauryl glucosyl 1-5%), EDTA-2Na 0.1-0.5%, citric acid 0.01-3%, essence 0.1-1.5%, Callicarpa nudiflora extract 1-20%, surplus is deionized water.
Method for making: by surfactant (as polyoxyethylenated alcohol sodium sulfate, lauryl alcohol sulfuric ester triethanolamine salt, dodecyldimethylammonium hydroxide inner salt, lauryl glucosyl), EDTA-2Na, deionized water mix homogeneously, be heated to 75 DEG C, treat to be all dissolved to transparence, stirring is cooled to 45 DEG C, add essence and Callicarpa nudiflora extract, it is 6-7 that citric acid is adjusted pH, stirs slow cooling to room temperature, to obtain final product.
, soap
Prescription: (%) meter by weight, soap base 70-90%, titanium dioxide 0.1-0.6%, EDTA-2Na 0.01-0.15%, essence 0.1-1.5%, Callicarpa nudiflora extract 1-20%, surplus is deionized water.
Method for making: by soap base and titanium dioxide, EDTA-2Na, essence, Callicarpa nudiflora extract, deionized water mix homogeneously, grind evenly by grinder, then through vacuum press strip cutting block forming.
, foot lotion
prescription:(%) meter by weight, surfactant 10-55%(is as polyoxyethylenated alcohol sodium sulfate 5-30%, dodecyldimethylammonium hydroxide inner salt 5-25%), salicylic acid 0.1-1%, glycerol 0.5-2%, white oil 0.5-2%, Callicarpa nudiflora extract 1-20%, essence 0.1-1.5%, surplus is deionized water.
Method for making: deionized water is heated to 65 DEG C, add while stirring surfactant (as polyoxyethylenated alcohol sodium sulfate, dodecyldimethylammonium hydroxide inner salt), salicylic acid, glycerol, white oil, be stirred to all and be uniformly dissolved, be cooled to 45 DEG C, add essence and Callicarpa nudiflora extract, stir slow cooling to room temperature, to obtain final product.
, bath foam
Prescription: weight (%) meter, surfactant 10-55%(is as polyoxyethylene lauryl ether sulfuric ester sodium salt 3-15%, lauryl alcohol sulfuric ester triethanolamine salt 4-25%, cocamido propyl betaine 3-15%), lanoline 0.1-1.5%, essence 0.1-1.5%, Callicarpa nudiflora extract 1-20%, surplus is deionized water.
Method for making: by surfactant (as polyoxyethylene lauryl ether sulfuric ester sodium salt, lauryl alcohol sulfuric ester triethanolamine salt, cocamido propyl betaine), lanoline, deionized water mix homogeneously, be heated to 75 DEG C, treat to be all dissolved to transparence, stirring is cooled to 45 DEG C, add essence and Callicarpa nudiflora extract, stir slow cooling to room temperature, to obtain final product.
, liquid detergent
Prescription: weight (%) meter, surfactant 10-55%(is as cocos nucifera oil alkanolamide 6501,3-25%, dodecylbenzene sodium sulfonate 7-30%), sodium hydroxide 0.1-1.5%, essence 0.1-1.5%, Callicarpa nudiflora extract 1-20%, citric acid 0.01-3%, surplus is deionized water.
Method for making: surfactant (as dodecylbenzene sodium sulfonate) and deionization waterside heating edge are stirred evenly to 75 DEG C, add sodium hydroxide to dissolve completely to it, after add surfactant (as cocos nucifera oil alkanolamide 6501), stirring is cooled to 45 DEG C, add essence and Callicarpa nudiflora extract, adding citric acid to adjust pH is 6-7, and the slow cooling that stirs, to room temperature, to obtain final product.
In the said goods, conventional surfactant includes but not limited to as polyoxyethylenated alcohol sodium sulfate, lauryl alcohol sulfuric ester triethanolamine salt, dodecyldimethylammonium hydroxide inner salt, lauryl glucosyl, polyoxyethylene lauryl ether sulfuric ester sodium salt, cocamido propyl betaine, cocos nucifera oil alkanolamide.
In the said goods, essence used is that laws and regulations allow the essence adding, and includes but not limited to Fructus Citri Limoniae essence, Citrua paradiai essence, rose essence, jasmin essence, lilac compound.
(3) Callicarpa nudiflora extract effect experiment
1, antibacterial experiment
(1) Callicarpa nudiflora extract antibacterial experiment
Test the antibacterial action of the Callicarpa nudiflora extract of preparing with minimum inhibitory concentration (MIC) and minimal bactericidal concentration (MBC) index evaluation the present invention to common bacterial strain by In Vitro Bacteriostasis.
Bacterium solution preparation: picking slant strains is inoculated in 20% N and soaks in juice culture medium, 37 DEG C of overnight incubation, then soak juice culture medium with 20% N bacterium liquid is diluted to 10cfu/ml, inoculation immediately.
MIC measures: adopt liquid tube serial dilution, soak juice culture medium sample is done to continuous two-fold dilution with 20% N.1.0 ml are added in sterilizing test tubes, and every pipe adds the fresh bacterium liquid of 0.05 ml standard, and establishes bacterial strain contrast and solvent matched group, cultivates 18~24 hours for 37 DEG C, observes bacterial growth situation, taking the high dilution of asepsis growth as MIC.
MBC measures: adopt plate streaking inocalation method, from be judged to the culture medium of adjacent two pipes of MIC and MIC, picking culture fluid is seeded on 10% serum MH bouillon agar flat board, cultivates 18~24 hours for 37 DEG C, taking the high dilution of clump count≤5 of growing as MBC.
Result of the test is in table 2.
Table 2 Callicarpa nudiflora extract In vitro Bactericidal Experiments result
The fresh medicinal substances extract of Callicarpa nudiflora prepared by the present invention and the dry medicinal substances extract of Callicarpa nudiflora all have staphylococcus aureus, escherichia coli, Bacillus typhi, streptococcus pneumoniae, bacillus pyocyaneus, group B streptococcus, γ-streptococcus and helicobacter pylori are all had to inhibition and killing action in various degree, and the fresh medicinal substances extract better effects if of Callicarpa nudiflora.
(2) product bacteriostasis antibiosis effect experiment of the present invention
The evaluation of the fungistatic effect of product of the present invention is carried out bacteriostatic test according to QB/T 2738-2005 " evaluation methodology of daily chemical products antibacterial bacteriostatic effect ", and test strain is pressed QB/T 2738-2005 " evaluation methodology of daily chemical products antibacterial bacteriostatic effect " for gold-coloured staphylococci, escherichia coli, Candida albicans, bacillus pyocyaneus.Antibacterial effect is evaluated as A2 level higher level (antibiotic rate >=50%), and fungistatic effect is for being B2 level higher level (bacteriostasis rate >=50%).
, skin irritation test
According to Ministry of Public Health " cosmetics health specification " 2007 editions, the sample of the present invention of censorship is carried out to toxicological experiment, under the experiment condition of Municipal Disease Control and Prevention Center, experimental result shows, Cavia porcellus repeatedly skin irritation test result is nonirritant.
(1) acute skin irritation experiment
Get 10 of Cavia porcelluss, spinal column diamond wool is cut, the each 3cm × 3cm in unhairing scope left and right, is coated in about submitted sample 0.5g on one side skin, with two layers of gauze and the covering of one deck cellophane, then uses nonirritant immobilization with adhesive tape, and opposite side in contrast.Carry out enclosed experiment, application 4h, after 4h, warm water cleans and removes residual given the test agent.
1 h, 24 h, 48 h, 72 h that remove after residual given the test agent observe the dermoreaction of smearing position, and according to the form below 3 carries out dermoreaction scoring.
(2) skin irritation test repeatedly
Get 10 of Cavia porcelluss, spinal column diamond wool is cut, the each 3cm × 3cm in unhairing scope left and right, application area is 2.5cm × 2.5cm, and submitted sample is coated in about submitted sample 0.5g on one side skin, opposite side is in contrast.Smear every day once, smear continuously 14 days.Since the 2nd day, smear front first cropping, water cleans removes residual receipts test agent, observes dermoreaction after 1h, and according to the form below 3 is marked.
Table 3 skin irritation reaction scoring
The integration of experimental result is zero, shows product nonirritant of the present invention.
The present invention is with respect to prior art, and tool has the following advantages and technique effect:
(1) inventor adds Callicarpa nudiflora in handwashing liquid, soap, foot lotion, bath foam, liquid detergent series daily use chemicals cleaning product first, by Callicarpa nudiflora extract and surfactant or other combination of active principles, strengthen bactericidal effect, nonirritant, prepared Callicarpa nudiflora series daily use chemicals cleaning product safety, effect uniqueness;
(2) the fresh medical material of the preferred Callicarpa nudiflora of the present invention is raw material, and its active component total flavones and content of luteolin are high compared with dry product, and extraction ratio improves greatly, be conducive to cost-saving, improve resource utilization.Directly taking Callicarpa nudiflora fresh goods as raw material, reduce the loss of active substance on the other hand, the effect that is conducive to improve active substance components group, the action effect of raising product.
Detailed description of the invention
the preparation of embodiment 1, Callicarpa nudiflora extract
Adopt the preparation of following either method, get one or more mixing wherein:
(1) adopt the fresh or dried feed of Callicarpa nudiflora, add water or rare alcohol or rare ketone solvent, heating extraction, extracting solution filters, and filtrate is concentrated, the dry Callicarpa nudiflora extract a that to obtain;
(2) adopt the fresh or dried feed of Callicarpa nudiflora, add water or rare alcohol or rare ketone solvent, heating extraction, extracting solution filters, and filtrate is passed through macroporous adsorbent resin column chromatography, wash cylinder with water, discard water lotion, then use 10%~90% ethanol elution, eluent filters, concentrated, be dried to obtain Callicarpa nudiflora extract b;
(3) the Callicarpa nudiflora raw material of fresh state, obtains pressed liquor and press residue through squeezing, and pressed liquor filters, and filtrate is concentrated, is dried to obtain Callicarpa nudiflora extract c;
(4) the Callicarpa nudiflora raw material of employing fresh state, obtains pressed liquor and press residue through squeezing, and press residue adds water or rare alcohol or rare ketone solvent, heating extraction, and extracting solution and pressed liquor merge, and filter, and filtrate is concentrated, is dried to obtain Callicarpa nudiflora extract d;
(5) the Callicarpa nudiflora raw material of employing fresh state, obtains pressed liquor and press residue through squeezing, and press residue adds water or rare alcohol or rare ketone solvent, heating extraction, extracting solution and pressed liquor merge, and filter, and filtrate is passed through macroporous adsorbent resin column chromatography, wash cylinder with water, discard water lotion, then use 10%~90% ethanol elution, eluent filters, concentrated, be dried to obtain Callicarpa nudiflora extract e;
(6) adopt fresh or dry Callicarpa nudiflora raw material, add water or rare alcohol or rare ketone decoction secondary, collecting decoction, filters, concentrated, carry out membrane filtration, first use ultrafiltration then nanofiltration, ceramic composite membrane and poly tetrafluoroethylene for membrane material, concentrated, be dried to obtain Callicarpa nudiflora f.
embodiment 2:
Get the fresh Callicarpa nudiflora leaf 1kg gathering October, add 2kg water and be broken into homogenate, squeezing, press residue adds 3kg water heating extraction, extracting solution and pressed liquor merge, filter, concentrated, be dried to obtain 124.7g extract, it is 12.47% that Callicarpa nudiflora extracts yield, recording general flavone content is 61.1mg/g, and content of luteolin is 0.74mg/g, and total tannin content 15.45 mg/g(are by fresh medical material).
embodiment 3
Get Callicarpa nudiflora leaf and twig 2.0kg(dry product), add rare ketone and decoct secondary, 10 times of amounts for the first time, decoct 2 hours, 8 times of amounts for the second time, decoct collecting decoction 1 hour, filter, be concentrated into 2000ml, carry out membrane filtration, first use ultrafiltration, then nanofiltration, ceramic composite membrane and poly tetrafluoroethylene for membrane material, concentrated, dry, obtain 290.1g Callicarpa nudiflora extract, it is 14.5% that Callicarpa nudiflora extracts yield, and recording general flavone content is 115.9mg/g, and content of luteolin is that 1.31mg/g(is by dry product).
embodiment 4
Get Callicarpa nudiflora leaf and twig 2.0kg(fresh goods), decoct with water secondary, each 10 times of amounts, decoct 2 hours, collecting decoction, filters, be concentrated into 2000ml, carry out membrane filtration, first use ultrafiltration, nanofiltration again, ceramic composite membrane and poly tetrafluoroethylene for membrane material, concentrated, dry, obtain 125.7g Callicarpa nudiflora extract, it is 6.28% that Callicarpa nudiflora extracts yield, recording general flavone content is 50.4mg/g, and content of luteolin is that 0.70mg/g(is by fresh goods).
embodiment 5
Get the fresh Callicarpa nudiflora leaf 1kg gathering August, add 2kg water and be broken into homogenate, squeezing, press residue adds the rare alcohol heating extraction of 3kg, and extracting solution and pressed liquor merge, and filters, filtrate, by macroporous adsorbent resin column chromatography, washes cylinder with water, discards water lotion, use 75% ethanol elution, de-liquid filters, concentrated again, be dried to obtain 88.5g extract, it is 8.85% that Callicarpa nudiflora extracts yield, and recording general flavone content is 58.7mg/g, and content of luteolin is that 0.72mg/g(is by fresh medical material).
embodiment 6
Get the fresh Callicarpa nudiflora leaf 1kg gathering October, heating extraction twice adds rare ketone 9kg at every turn, extracts 2 hours, merging filtrate, filter, concentrated, be dried to obtain 93.7g extract, it is 9.37% that Callicarpa nudiflora extracts yield, recording general flavone content is 49.5mg/g, and content of luteolin is 0.75mg/g, and total tannin content 13.87 mg/g(are by fresh medical material).
embodiment 7
Get Callicarpa nudiflora leaf and twig 2.0kg(dry product), heating extraction twice adds rare alcohol 10kg at every turn, extracts 2 hours, merging filtrate, filter, concentrated, be dried to obtain 485.8g extract, it is 24.3% that Callicarpa nudiflora extracts yield, recording general flavone content is 104.7mg/g, and content of luteolin is 1.29mg/g, and total tannin content 38.4 mg/g(are by dry product).
embodiment 8, handwashing liquid
Prescription: (%) meter by weight, polyoxyethylenated alcohol sodium sulfate 10%, lauryl alcohol sulfuric ester triethanolamine salt 8%, dodecyldimethylammonium hydroxide inner salt 4%, lauryl glucosyl 4%, EDTA-2Na 0.1%, citric acid 0.05-1%, essence 1%, Callicarpa nudiflora extract 8%, surplus is deionized water.
Method for making: by polyoxyethylenated alcohol sodium sulfate, lauryl alcohol sulfuric ester triethanolamine salt, dodecyldimethylammonium hydroxide inner salt, lauryl glucosyl, EDTA-2Na, deionized water mix homogeneously, be heated to 75 DEG C, treat to be all dissolved to transparence, stirring is cooled to 45 DEG C, add essence and Callicarpa nudiflora extract, it is 6-7 that citric acid is adjusted pH, stirs slow cooling to room temperature, to obtain final product.
embodiment 9, soap
Prescription: (%) meter by weight, soap base 88%, titanium dioxide 0.5%, EDTA-2Na 0.1%, essence 0.2%, Callicarpa nudiflora extract 8%, surplus is deionized water.
Method for making: by soap base and titanium dioxide, EDTA-2Na, essence, Callicarpa nudiflora extract, deionized water mix homogeneously, grind evenly by grinder, then through vacuum press strip cutting block forming.
embodiment 10, foot lotion
prescription:(%) meter by weight, polyoxyethylenated alcohol sodium sulfate 6%, dodecyldimethylammonium hydroxide inner salt 10%, salicylic acid 1%, glycerol 2%, white oil 2%, Callicarpa nudiflora extract 10%, essence 0.5%, deionized water surplus etc.
Method for making: deionized water is heated to 65 DEG C, add while stirring polyoxyethylenated alcohol sodium sulfate, dodecyldimethylammonium hydroxide inner salt, salicylic acid, glycerol, white oil, be stirred to all and be uniformly dissolved, be cooled to 45 DEG C, add essence and Callicarpa nudiflora extract, stir slow cooling to room temperature, to obtain final product.
embodiment 11, bath foam
Prescription: (%) meter by weight, polyoxyethylene lauryl ether sulfuric ester sodium salt 14%, lauryl alcohol sulfuric ester triethanolamine salt 16%, cocamido propyl betaine 8%, lanoline 1%, essence 0.8%, Callicarpa nudiflora extract 4%, surplus is deionized water.
Method for making: by polyoxyethylene lauryl ether sulfuric ester sodium salt, lauryl alcohol sulfuric ester triethanolamine salt, cocamido propyl betaine, lanoline, deionized water mix homogeneously, be heated to 75 DEG C, treat to be all dissolved to transparence, stirring is cooled to 45 DEG C, add essence and Callicarpa nudiflora extract, stir slow cooling to room temperature, to obtain final product.
embodiment 12, liquid detergent
Prescription: (%) meter by weight, cocos nucifera oil alkanolamide 6501,3%, dodecylbenzene sodium sulfonate 8%, sodium hydroxide 1%, essence 0.2%, Callicarpa nudiflora extract 10%, citric acid 0.05-1%, surplus is deionized water.
Method for making: dodecylbenzene sodium sulfonate and deionization waterside heating edge are stirred evenly to 75 DEG C, add sodium hydroxide to dissolve completely to it, after add cocos nucifera oil alkanolamide 6501, stirring is cooled to 45 DEG C, add essence and Callicarpa nudiflora extract, adding citric acid to adjust pH is 6-7, and the slow cooling that stirs, to room temperature, to obtain final product.