CN1314703C - A kind of preparation technology of saponin and its application - Google Patents
A kind of preparation technology of saponin and its application Download PDFInfo
- Publication number
- CN1314703C CN1314703C CNB2005100116738A CN200510011673A CN1314703C CN 1314703 C CN1314703 C CN 1314703C CN B2005100116738 A CNB2005100116738 A CN B2005100116738A CN 200510011673 A CN200510011673 A CN 200510011673A CN 1314703 C CN1314703 C CN 1314703C
- Authority
- CN
- China
- Prior art keywords
- saponin
- pericarp
- extraction
- weight ratio
- extract
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229930182490 saponin Natural products 0.000 title claims abstract description 117
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 115
- 150000007949 saponins Chemical class 0.000 title claims abstract description 115
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000005516 engineering process Methods 0.000 title description 13
- 238000000605 extraction Methods 0.000 claims abstract description 69
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000575 pesticide Substances 0.000 claims abstract description 7
- 239000002453 shampoo Substances 0.000 claims abstract description 6
- 239000003599 detergent Substances 0.000 claims abstract description 4
- 235000013399 edible fruits Nutrition 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 18
- 239000013078 crystal Substances 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 15
- 239000012535 impurity Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 238000002425 crystallisation Methods 0.000 claims description 10
- 230000008025 crystallization Effects 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 7
- 239000000284 extract Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 5
- 238000013467 fragmentation Methods 0.000 claims description 4
- 238000006062 fragmentation reaction Methods 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 235000017709 saponins Nutrition 0.000 claims 20
- 241000220479 Acacia Species 0.000 claims 3
- 235000010643 Leucaena leucocephala Nutrition 0.000 claims 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 2
- 229910052742 iron Inorganic materials 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 5
- 241000931143 Gleditsia sinensis Species 0.000 description 19
- 229960000935 dehydrated alcohol Drugs 0.000 description 16
- 239000003814 drug Substances 0.000 description 16
- 238000005238 degreasing Methods 0.000 description 15
- 239000003905 agrochemical Substances 0.000 description 12
- 229960004756 ethanol Drugs 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- 150000001408 amides Chemical class 0.000 description 8
- 238000012216 screening Methods 0.000 description 8
- 244000068988 Glycine max Species 0.000 description 6
- 235000010469 Glycine max Nutrition 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- ZXQYGBMAQZUVMI-UNOMPAQXSA-N cyhalothrin Chemical compound CC1(C)C(\C=C(/Cl)C(F)(F)F)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-UNOMPAQXSA-N 0.000 description 5
- 239000003085 diluting agent Substances 0.000 description 5
- 230000008030 elimination Effects 0.000 description 5
- 238000003379 elimination reaction Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 235000014347 soups Nutrition 0.000 description 5
- 241001124076 Aphididae Species 0.000 description 4
- 235000011430 Malus pumila Nutrition 0.000 description 4
- 235000015103 Malus silvestris Nutrition 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000007865 diluting Methods 0.000 description 4
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 4
- 239000010813 municipal solid waste Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 235000013311 vegetables Nutrition 0.000 description 4
- 244000141359 Malus pumila Species 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 229920002907 Guar gum Polymers 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 208000003251 Pruritus Diseases 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- -1 acetone saponin Chemical class 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000003110 anti-inflammatory effect Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 239000000665 guar gum Substances 0.000 description 2
- 229960002154 guar gum Drugs 0.000 description 2
- 235000010417 guar gum Nutrition 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 235000014666 liquid concentrate Nutrition 0.000 description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000004083 survival effect Effects 0.000 description 2
- 239000012747 synergistic agent Substances 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- 244000070406 Malus silvestris Species 0.000 description 1
- 241000237502 Ostreidae Species 0.000 description 1
- RGDJCYRXKJVXKD-UHFFFAOYSA-N Saponin 3 Natural products COC(=O)C1(C)CCC2(CCC3(C)C(=CCC4C5(C)CCC(OC6OC(CO)C(O)C(O)C6OC7OC(CO)C(O)C(O)C7O)C(C)(C)C5CCC34C)C2C1)C(=O)O RGDJCYRXKJVXKD-UHFFFAOYSA-N 0.000 description 1
- 230000036592 analgesia Effects 0.000 description 1
- 239000006286 aqueous extract Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- WCMJLEULXWUCRF-UHFFFAOYSA-N emarginatoside B Natural products C12CC(C)(C)CCC2(C(O)=O)CCC(C2(CCC3C4(CO)C)C)(C)C1=CCC2C3(C)CCC4OC1OC(CO)C(O)C(O)C1OC1OC(CO)C(O)C(O)C1O WCMJLEULXWUCRF-UHFFFAOYSA-N 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000003845 household chemical Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 235000020636 oyster Nutrition 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229940095673 shampoo product Drugs 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229930182493 triterpene saponin Natural products 0.000 description 1
- 235000012773 waffles Nutrition 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Landscapes
- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
本发明属林产化工与应用化学领域。本发明公开了一种适合皂荚皂素制备的新型高效简洁工艺，其特征在于，采用无水乙醇萃取分离。并公开了其在农药、洗涤剂、洗发液中的应用。The invention belongs to the field of forest product chemical industry and applied chemistry. The invention discloses a novel high-efficiency and concise process suitable for the preparation of saponin, which is characterized in that absolute ethanol is used for extraction and separation. It also discloses its application in pesticides, detergents and shampoos.
Description
Technical field
The invention belongs to forest chemical and applied chemistry field, relate to a kind of Gleditisia sinensis Saponin preparation technology and the application in agricultural chemicals, washing composition, shampoo thereof.
Background technology
Gleditisia sinensis Saponin (Gleditisia sinensis Saponin) claim gleditschiasaponin again, is the pentacyclic triterpene saponin that is made of fundamental units such as aglucon, sugared body and organic acids.Therefore being made of hydrophilic sugared body and hydrophobic coordinating group in the Gleditisia sinensis Saponin molecule, having the active character of kinds of surface such as emulsification, dispersion, wetting, decontamination, foaming, is a kind of natural nonionic surface active agent.In addition, Gleditisia sinensis Saponin also have tangible anti-inflammatory, impermeabilisation ability and anti-inflammatory, eliminate the phlegm, effect such as analgesia, sterilization, desinsection.Therefore, Gleditisia sinensis Saponin can be used for making products such as various types of emulsifying agents, washing composition, sterilant or sterilant, is the natural surface active agent that has DEVELOPMENT PROSPECT in current household chemicals, cosmetic skin care, medicine and the pesticide industry.
The Gleditsia officinalis well developed root system, drought-enduring water saving, solid good, be the desirable ecological seeds of building farmland shelter, soil and water conservation forest and town and country view woods.There is wild Chinese honey locust woods in Shaanxi, Henan, Hebei, Sichuan, and artificial Chinese honey locust woods has been developed in these areas again at present, and cultivated area is above 300,000 mu.Seed content 15-30% in the full fruit of Chinese honey locust is rich in high-quality polysaccharide glue in the seed, its preparation technology has declared patent of invention (CN03132340.5); Pericarp content is 70-85%, and saponin content is up to 35% in the pericarp, and the output of pericarp is 3-5 times of seed production.Therefore, the development and use of Chinese honey locust pericarp have decisive meaning to the efficient utilization and the comprehensive utilization of Chinese honey locust resource.In the 30 multinomial patents of relevant Chinese honey locust, mainly directly utilize Chinese honey locust raw material or the composite Chinese medicine of its aqueous extract, agricultural chemicals and articles for washing (CN1424102A, CN1301533A, CN1060313C etc.), do not see patent report relevant for Gleditisia sinensis Saponin preparation technology.
The production of saponin mainly contains two kinds of water extraction and organic solvent methods.Water extraction is produced, and its production technique, production unit are simple, but have big, the conventional separation difficulty of water treatment amount, shortcoming such as product purity is low, energy consumption is big.Organic solvent method mainly is to utilize the pure water solvent contain 70-95% that raw material is extracted, this technology have extraction efficiency height, quality product better, be suitable for advantage such as suitability for industrialized production, but complex process, investment is big, product needs further purification.
Summary of the invention
The objective of the invention is to propose a kind of new and effective succinct technology and the application in agricultural chemicals, washing composition, shampoo thereof of suitable Gleditisia sinensis Saponin preparation.
The invention discloses a kind of technology for preparing Gleditisia sinensis Saponin, it is characterized in that adopting the dehydrated alcohol extracting and separating.
Technology of the present invention, it comprises the steps:
(1) with the full fruit of Chinese honey locust, the cleaning impurity elimination;
(2) full fruit is carried out fragmentation, remove seed;
(3) pulverize pericarp;
(4) fat-soluble component in the adding extraction agent extracting and separating pericarp;
(5) the degreasing pericarp is used dehydrated alcohol extracting and separating saponin;
(6) concentrated extract makes the saponin crystallization;
(7) saponin crystal vacuum filtration, laundry soap cellulose crystal, drying.
Preferably, it comprises the steps:
(1) the full fruit of Chinese honey locust of selection moisture content≤8%, cleaning impurity elimination, trash content≤0.5%;
(2) full fruit is carried out fragmentation, remove seed, seed clearance 〉=95%;
(3) pulverize pericarp, the pericarp granularity of crushing screening is 2-5mm;
(4) fat-soluble component in the adding extraction agent extracting and separating pericarp, the weight proportion of extraction agent and pericarp is 2-7: 1, the extraction time is 2-8 hour;
(5) the degreasing pericarp is used dehydrated alcohol extracting and separating saponin, and the weight proportion of dehydrated alcohol and degreasing pericarp is 3-9: 1, and extraction temperature is 40-80 ℃, the extraction time is 3-9 hour;
(6) concentrated extract makes the saponin crystallization, and saponin and ethanol weight ratio are 1: 0.3-1.5, and the saponin Tc is 5-30 ℃;
(7) saponin crystal vacuum filtration, laundry soap cellulose crystal, washing composition consumption are 2 times of saponin weight, drying, temperature 50-100 ℃.
Preferred, it comprises the steps:
(1) the full fruit of Chinese honey locust of selection moisture content≤8%, the cleaning impurity elimination, trash content≤0.5% does not contain ironware impurity;
(2) full fruit is carried out fragmentation, remove seed, seed clearance 〉=95%;
(3) pulverize pericarp, the pericarp granularity of crushing screening is 2-5mm;
(4) adding soybean extracting solvent no.6 (boiling range 60-90 ℃) or petroleum ether extraction separate the fat-soluble component in the pericarp, and the weight proportion of extraction agent and pericarp is 3.5: 1, and the extraction time is 4 hours;
(5) the degreasing pericarp is used dehydrated alcohol extracting and separating saponin, and the weight proportion of dehydrated alcohol and degreasing pericarp is 4.5: 1, and extraction temperature is 60-70 ℃, and the extraction time is 5 hours;
(6) concentrated extract makes the saponin crystallization, and saponin and ethanol weight ratio are 1: 0.8, and the saponin Tc is 15 ℃;
(7) saponin crystal vacuum filtration, with washing with acetone saponin crystal, the washing composition consumption is 2 times of saponin weight, divides three washings, drying, 80 ℃ of temperature.
Details are as follows for described technology:
(1) ingredient requirement: the full fruit of Chinese honey locust moisture content≤8%, after the cleaning impurity elimination, trash content≤0.5% does not contain ironware impurity;
(2) adopt bar disintegrator or beater disintegrating machine that full fruit is carried out Mechanical Crushing, remove seed, seed clearance 〉=95% by screening or gravity.
(3) pericarp is pulverized and is adopted beater grinder or bar disintegrator, and the pericarp granularity of crushing screening is 2-5mm.
(4) soybean extracting solvent no.6 (Nanjing petrochemical industry limited liability company) (boiling range 60-90 ℃) or petroleum ether extraction separate the fat-soluble component in the pericarp, and the weight proportion of extraction agent and pericarp is 2-7: 1, and best proportioning is 3.5: 1; The extraction time is 2～8 hours, and optimum extraction time is 4 hours.
(5) the degreasing pericarp is used dehydrated alcohol extracting and separating saponin, and the weight proportion of dehydrated alcohol and degreasing pericarp is 3-9: 1, and best proportioning is 4.5: 1; Extraction temperature is 40-80 ℃, and best extraction temperature is 60-70 ℃; The extraction time is 3-9 hour, and optimum extraction time is 5 hours.
(6) extraction liquid concentrates, and saponin and ethanol weight ratio are 1: 0.3-1.5, optimum weight ratio are 1: 0.8; The saponin Tc is 5-30 ℃, and best Tc is 15 ℃; Extraction liquid concentrate to reclaim the alcohol solvent that obtains after no aquation processing as the extraction agent reuse.
(7) the saponin crystal filters and adopts vacuum filter, all reclaims alcohol solvent; With washing with acetone saponin crystal, the washing composition consumption is 2 times of saponin weight, divides three washings; Dry van-type dryer or the airflow dryer of adopting of saponin, drying temperature is 50-100 ℃, the optimum drying temperature is 80 ℃.
The invention provides the application of Gleditisia sinensis Saponin in agricultural chemicals of described prepared.
With 24.3% (weight percent, down with) to kill vegetable aphid worm effect basic identical for 2500 times of Gleditisia sinensis Saponin and the 0.7% cyhalothrin mixed dilutings effect of killing the vegetable aphid worm and 2500 times of 2.5% cyhalothrin mixed dilutings, can save 72% cyhalothrin consumption behind the use Gleditisia sinensis Saponin;
After in 2500 times of diluents of Bristol gram, adding the Gleditisia sinensis Saponin of 1500-3500mg/L, medicine liquid droplet the apple tree blade just, the back side, its contact angle has reduced 15.2-24.6% and 13.5-21.3% respectively, the deposition of Bristol gram soup on the Folium Mali pumilae surface behind the adding 2500mg/L saponin can improve 27.4%, reach identical prevention effect, can reduce Bristol and restrain 90.5% of former survival dose, reduce the agricultural chemicals use cost greatly, also reduce the pollution of agricultural chemicals significantly environment.
After adding Gleditisia sinensis Saponin in the agricultural chemicals, improved soup at the adhesive ability of plant surface and target organisms, moistening spread ability and effective precipitation, and then the result of use of raising agricultural chemicals, so Gleditisia sinensis Saponin both can be used as biological pesticide, good especially pesticide synergistic agent.
The Gleditisia sinensis Saponin that the invention provides described prepared is in detergent application.
Silk, woollen detergent formulation (weight percent): Gleditisia sinensis Saponin 2-5%, diglycollic amide (6501) 5-7%, dodecyl alcohol polyoxyethylene ether sulfate (AES) 8-11%, sodium sulfonate 4-6%, carboxymethyl cellulose (CMC) 1-2%, essence 0.5%, deionized water adds to 100%.
The invention provides the application of Gleditisia sinensis Saponin in shampoo of described prepared.
Shampoo prescription (weight percent): Gleditisia sinensis Saponin 1-4%, AESA (AESA) 8-12%, diglycollic amide (6501) 1-3%, CAB (CAB-30) 3-7%, citric acid 0.1-1%, cation guar gum 0.1-0.5%, pearly-lustre dibasic acid esters 1-3%, silicone oil emulsion 0.5-3%, pruritus 0.5%, essence 0.5%, deionized water adds to 100%.
Chinese honey locust is made up of seed and pericarp two portions by full fruit.From the full fruit of Chinese honey locust, prepare saponin, because saponin is present in the pericarp, at first pericarp is separated with seed with the method for mechanical separation, both avoided in the seed each composition to preparing the influence of saponin process, separate the raw material that the seed that obtains can be used as preparation polysaccharide glue, kill two birds with one stone.Fat-soluble component is to the influence of preparation saponin in the pericarp in order to remove, and the present invention adopts soybean extracting solvent no.6 extraction pericarp.The present invention adopts the saponin in the dehydrated alcohol extraction pericarp, test shows that the size of water content in the organic solvent directly has influence on the purity of product, water content within the specific limits is big more, though the disposable extraction yield of product slightly improves, but product is difficult more with separating of extraction slag, and therefore saponin purity also reduce, and causes the purifying technique of product to become complicated.Consider the dissolution characteristics of main component in ethanol in the pericarp, be that saponin slightly is dissolved in cold ethanol and is soluble in hot ethanol, the dissolution degree of all the other compositions in ethanol is little of ignoring, adopting the dehydrated alcohol of heat is solvent, the reflux extraction Gleditisia sinensis Saponin, and filtered while hot makes the sharp separation of saponin product and raw material, the saponin extraction and purification carries out synchronously, and product yield and purity all is significantly improved, and preparation technology is efficiently succinct.The saponin xln can make the Gleditisia sinensis Saponin finished product through washing with acetone, drying, and the highest yield of saponin can reach 33% in the pericarp, and extraction yield is greater than 92%, and product purity is greater than 96%.
Description of drawings
Fig. 1 Gleditisia sinensis Saponin preparation technology of the present invention schema
Embodiment
Embodiment 1:
Select the full fruit of Chinese honey locust of moisture content≤8%, after the cleaning impurity elimination, trash content≤0.5% does not contain ironware impurity; Adopt bar disintegrator that full fruit is carried out Mechanical Crushing, separate seed, seed separation and Extraction rate 〉=95%; With the Chinese honey locust pericarp behind the separation seed, through the beater grinder crushing screening, obtaining granularity is 2～3mm pericarp particle.With the fat-soluble component in soybean extracting solvent no.6 (Nanjing petrochemical industry limited liability company) the extracting and separating pericarp, the weight proportion of extraction agent and pericarp is 3.5: 1, and the extraction time is 5 hours.The degreasing pericarp is used dehydrated alcohol extracting and separating saponin, and the weight proportion of dehydrated alcohol and degreasing pericarp is 4: 1, and extraction temperature is 60 ℃, and the extraction time is 5 hours.Extraction liquid is concentrated into saponin and the ethanol weight ratio is 1: 0.8 o'clock, 15 ℃ of following crystallizations.The saponin crystal filters through vacuum filter, and 2 times of washing with acetones and van-type drier obtain the Gleditisia sinensis Saponin product.Measure counting yield yield, saponin purity and saponin extraction yield respectively, it the results are shown in Table 1.
Embodiment 2:
With the Chinese honey locust pericarp behind the separation seed, through the beater grinder crushing screening, obtaining granularity is 0.5-2mm pericarp particle.With the fat-soluble component in soybean extracting solvent no.6 (Nanjing petrochemical industry limited liability company) the extracting and separating pericarp, the weight proportion of extraction agent and pericarp is 7: 1, and the extraction time is 6 hours.The degreasing pericarp is used dehydrated alcohol extracting and separating saponin, and the weight proportion of dehydrated alcohol and degreasing pericarp is 8: 1, and extraction temperature is 60 ℃, and the extraction time is 8 hours.Extraction liquid is concentrated into saponin and the ethanol weight ratio is 1: 1 o'clock, 15 ℃ of following crystallizations.The saponin crystal filters through vacuum filter, and 2 times of washing with acetones and van-type drier obtain the Gleditisia sinensis Saponin product.Measure counting yield yield, saponin purity and saponin extraction yield respectively, it the results are shown in Table 1.
Embodiment 3:
With the Chinese honey locust pericarp behind the separation seed, through the beater grinder crushing screening, obtaining granularity is 5-6mm pericarp particle.With the fat-soluble component in the petroleum ether extraction separation pericarp, the weight proportion of extraction agent and pericarp is 4: 1, and the extraction time is 3 hours.The degreasing pericarp is used dehydrated alcohol extracting and separating saponin, and the weight proportion of dehydrated alcohol and degreasing pericarp is 5: 1, and extraction temperature is 60 ℃, and the extraction time is 4 hours.Extraction liquid is concentrated into saponin and the ethanol weight ratio is 1: 1 o'clock, 15 ℃ of following crystallizations.The saponin crystal filters through vacuum filter, and 2 times of washing with acetones and van-type drier obtain the Gleditisia sinensis Saponin product.Measure counting yield yield, saponin purity and saponin extraction yield respectively, it the results are shown in Table 1.
Reference examples 1:
With the Chinese honey locust pericarp behind the separation seed, through the beater grinder crushing screening, obtaining granularity is 2-3mm pericarp particle.With the fat-soluble component in the soybean extracting solvent no.6 extracting and separating pericarp, the weight proportion of extraction agent and pericarp is 3.5: 1, and the extraction time is 5 hours.The degreasing pericarp is with 80% alcohol-water extracting and separating saponin, and the weight proportion of aqueous ethanolic solution and degreasing pericarp is 5: 1, and extraction temperature is 60 ℃, and the extraction time is 5 hours.Extraction liquid is concentrated into saponin and the ethanol weight ratio is 1: 1 o'clock, 15 ℃ of following crystallizations.The saponin crystal filters through vacuum filter, and 2 times of washing with acetones and van-type drier obtain the Gleditisia sinensis Saponin product.Measure counting yield yield, saponin purity and saponin extraction yield respectively, it the results are shown in Table 1.
The product yield of the different embodiment conditions of table 1, saponin purity and saponin extraction yield
| Product yield (%) | Saponin purity (%) | Saponin extraction yield (%) | |
| Embodiment 1 | 33.2 | 98.6 | 93.2 |
| Embodiment 2 | 33.5 | 96.5 | 92.8 |
| Embodiment 3 | 31.7 | 97.4 | 88.2 |
| Reference examples 1 | 34.0 | 87.2 | 84.7 |
Application Example 1:
Experimental pharmacy:
Medicament 1: with 2500 times of 24.3% Gleditisia sinensis Saponin and 0.7% cyhalothrin (the rich day chemical company limited in Wuhan) mixed dilutings.
2500 times of medicament 2:2.5% cyhalothrin (the rich day chemical company limited in Wuhan) mixed dilutings.
Table 2 is killed vegetable aphid worm effect
| Medicament 1 | Medicament 2 | |
| Vegetable aphid worm killing rate | 98.7％ | 99.2％ |
Application Example 2:
Experimental pharmacy:
Medicament 1: the Gleditisia sinensis Saponin that in 2500 times of diluents of Bristol gram, adds 1500mg/L
Medicament 2: the Gleditisia sinensis Saponin that in 2500 times of diluents of Bristol gram, adds 2500mg/L
Medicament 3: the Gleditisia sinensis Saponin that in 2500 times of diluents of Bristol gram, adds 3500mg/L
Respectively with medicament 1,2,3 medicine liquid droplets the apple tree blade just, the back side, its contact angle reduced rate respectively sees Table 3.
Soup contact angle reduced rate behind the adding Gleditisia sinensis Saponin in the table 3 Bristol gram diluent
| Medicament 1 | Medicament 2 | Medicament 3 | |
| Apple tree blade front | 15.2％ | 18.1％ | 24.6％ |
| The apple tree blade back side | 13.5％ | 17.9％ | 21.3％ |
Medicament 2 can make the deposition of Bristol gram soup on the Folium Mali pumilae surface improve 27.4%, reaches identical prevention effect, can reduce Bristol and restrain 90.5% of former survival dose.
The result show in the agricultural chemicals add Gleditisia sinensis Saponin after, improved soup at the adhesive ability of plant surface and target organisms, moistening spread ability and effective precipitation, and then the result of use of raising agricultural chemicals, reduce the agricultural chemicals use cost greatly, also reduced the pollution of agricultural chemicals significantly to environment., so Gleditisia sinensis Saponin both can be used as biological pesticide, good especially pesticide synergistic agent.
Application Example 3:
Carboxymethyl cellulose (CMC) 1% (weight percent) is added in the deionized water, be stirred to fully and disperse.Add dodecyl alcohol polyoxyethylene ether sulfate (AES) 10% (middle waffle worker company limited) successively, sodium sulfonate 4.5% is heated to 70 ℃, stirring and dissolving; Add diglycollic amide (6501) 5% (Haikou rising sun Chinese workers trade company limited), insulation 50min; Be cooled to 50 ℃, add Gleditisia sinensis Saponin 4%, essence 0.5% etc., promptly make silk, woollen Betengent product after stirring.
Application Example 4:
Cation guar gum amendment 0.3% (weight percent) is added in the deionized water, be stirred to fully and disperse.Add 0.2% citric acid, CAB (CAB-30) 5% (Shanghai through big chemical industry company limited), AESA (AESA) 10% (Huifeng, Ezhou auxiliary agent company limited) successively, be heated to 75 ℃, stirring and dissolving; Add pearly-lustre dibasic acid esters 3%, diglycollic amide (6501) 2% (Haikou rising sun Chinese workers trade company limited), insulation 30min; Be cooled to 50 ℃, add Gleditisia sinensis Saponin 3%, silicone oil emulsion 2%, pruritus 0.5%, essence 0.5% etc., promptly make the shampoo product after stirring.The key technical indexes that mensuration obtains is as follows: outward appearance is an oyster white, pH 6.0-7.0, viscosity (mPa.s) 〉=500, foam (mm) 〉=100, thermotolerance (no layering and precipitating metachromatism behind 48 ℃ of 24h), winter hardiness (returning to the room temperature no change behind 20 ℃ of 24h).
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100116738A CN1314703C (en) | 2005-04-29 | 2005-04-29 | A kind of preparation technology of saponin and its application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100116738A CN1314703C (en) | 2005-04-29 | 2005-04-29 | A kind of preparation technology of saponin and its application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1696145A CN1696145A (en) | 2005-11-16 |
| CN1314703C true CN1314703C (en) | 2007-05-09 |
Family
ID=35349053
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100116738A Expired - Fee Related CN1314703C (en) | 2005-04-29 | 2005-04-29 | A kind of preparation technology of saponin and its application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1314703C (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AR052448A1 (en) * | 2005-12-28 | 2007-03-21 | Ideasupply Com Argentina S A | EXTRACT OF THE SHEATH WITHOUT SEEDS OF GLEDITSIA AMORPHOIDES AND ITS USE AS AN ASSISTANT IN AGRO |
| CN102273450A (en) * | 2010-06-12 | 2011-12-14 | 甘肃省农业科学院植物保护研究所 | Plant source pesticide synergist and preparation method thereof |
| CN103073599B (en) * | 2013-01-18 | 2015-01-28 | 北京林业大学 | Concentrating and extracting method for saponins |
| CN103059093B (en) * | 2013-01-18 | 2015-05-20 | 北京林业大学 | Method for preparing saponin by vacuum digestion |
| CN104757025B (en) * | 2014-01-02 | 2018-04-06 | 甘玉祥 | A kind of wide spectrum expelling worm plant and agricultural chemicals product |
| CN103881838B (en) * | 2014-03-07 | 2016-09-21 | 北京林业大学 | Fructus Sapindi Mukouossi fluid composition, dish washing detergent containing Fructus Sapindi Mukouossi fluid composition |
| CN105342932B (en) * | 2015-12-11 | 2019-03-05 | 中华全国供销合作总社南京野生植物综合利用研究院 | A kind of all natural multifunctional liquid soap and its production method containing carboxymethyl chitosan |
| CN107033197B (en) * | 2017-04-28 | 2020-06-09 | 武鸣馨艺荣牛大力中草药种植专业合作社 | A method for extracting saponin from Gleditsia sinensis |
| CN108478494A (en) * | 2018-06-08 | 2018-09-04 | 中华全国供销合作总社南京野生植物综合利用研究所 | A kind of all natural shampoo |
| CN113583766A (en) * | 2021-08-18 | 2021-11-02 | 广州德谷个人护理用品有限公司 | Formula and preparation method of laundry detergent containing gleditschia horrida saponin |
| CN113599322A (en) * | 2021-08-18 | 2021-11-05 | 中华全国供销合作总社南京野生植物综合利用研究所 | A shampoo formula containing Gleditsia sinensis saponin and its preparation method |
| CN113549502A (en) * | 2021-08-18 | 2021-10-26 | 中华全国供销合作总社南京野生植物综合利用研究所 | Formula and preparation method of liquid detergent containing gleditschia horrida saponin |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1054788A (en) * | 1990-03-09 | 1991-09-25 | 华东地质学院应用技术研究所 | Process for extracting grease and tea saponin by one-step leaching of cake dregs |
-
2005
- 2005-04-29 CN CNB2005100116738A patent/CN1314703C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1054788A (en) * | 1990-03-09 | 1991-09-25 | 华东地质学院应用技术研究所 | Process for extracting grease and tea saponin by one-step leaching of cake dregs |
Non-Patent Citations (6)
| Title |
|---|
| 以无水乙醇为提取剂的茶皂素提取方法研究 杨坤国等，湖南民蔟学院学报，第18卷第3期 2000 * |
| 天然茶皂素的提取及泡沫性能 尹忠等，应用化工，第31卷第4期 2002 * |
| 无水乙醇法提纯粗茶皂素初探 卢仁杰等，上铙师专学报，第3卷 1996 * |
| 茶皂素提取与精制方法的改进研究 杨坤国等，林产化学与工业，第21卷第2期 2001 * |
| 茶皂素的精制及应用 章湘云等，广西化工，第27卷第2期 1998 * |
| 茶皂素的精制及应用 章湘云等，广西化工，第27卷第2期 1998;茶皂素提取与精制方法的改进研究 杨坤国等，林产化学与工业，第21卷第2期 2001;天然茶皂素的提取及泡沫性能 尹忠等，应用化工，第31卷第4期 2002;无水乙醇法提纯粗茶皂素初探 卢仁杰等，上铙师专学报，第3卷 1996;以无水乙醇为提取剂的茶皂素提取方法研究 杨坤国等，湖南民蔟学院学报，第18卷第3期 2000 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1696145A (en) | 2005-11-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1314703C (en) | A kind of preparation technology of saponin and its application | |
| CN103951722B (en) | A method for jointly extracting hesperidin and pectin from citrus peel | |
| CN103952245A (en) | Natural detergent and preparation method and application thereof | |
| CN103088101B (en) | Method for extracting natural saponin and biosurfactant composite product | |
| CN101607997B (en) | Method for extracting polysaccharide compound of traditional Chinese medicine cassia seed | |
| CN104921998A (en) | Process for simultaneously extracting pigments, saponins and polysaccharides of sapindus, and preparation and application of saponins of sapindus | |
| CN101955548B (en) | Method for extracting tribulus terrestris polysaccharide with assistance of enzyme method | |
| CN101497642A (en) | Method for directly extracting tea saponin from tea seeds | |
| CN1507429A (en) | Extract from lupine seed pods containing lupeol | |
| CN108997443A (en) | A kind of method that microbial fermentation extracts saponin(e in plant | |
| CN102807570B (en) | The fragrant fruit of a kind ofization prepares the method for ellagic acid | |
| CN105622777A (en) | Technology for extracting pectin from premna microphylla turca | |
| CN103059093B (en) | Method for preparing saponin by vacuum digestion | |
| CN105541959B (en) | A kind of extraction method of turmeric saponin | |
| CN101899120B (en) | Method for refining jujube polysaccharide | |
| CN104844683A (en) | Method for extracting peony saponin from peony seed meal | |
| CN110013506A (en) | Extraction method and application of effective bactericidal components of Houttuynia cordata | |
| CN103319628B (en) | The method of chondroitin sulfate is prepared in super-voltage micro jet ultrafiltration | |
| CN110025691A (en) | A kind of compound houttuynia cordata preparation and preparation method and application | |
| CN101880203B (en) | Vegetable foliar biological fertilizer and preparation method thereof | |
| CN109453071A (en) | A kind of rosemary bacteriostatic hand sanitizer and preparation method thereof | |
| CN101240293B (en) | Bran extract and cleansing composition comprising bran extract and preparation method thereof | |
| CN103382230B (en) | From the method for extracting pectin from watermelon peel | |
| CN107022012A (en) | A kind of extracting method of tealeaves alcohol soluble protein | |
| CN102321715A (en) | Method for comprehensively preparing wheat polypeptide, wheat gliadin and wheat bran massage particles and application of wheat polypeptide, wheat gliadin and wheat bran massage particles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070509 Termination date: 20140429 |