CN103305580A - Method for preparing collagen peptide from mammal skin and bone - Google Patents
Method for preparing collagen peptide from mammal skin and bone Download PDFInfo
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- CN103305580A CN103305580A CN2013102771998A CN201310277199A CN103305580A CN 103305580 A CN103305580 A CN 103305580A CN 2013102771998 A CN2013102771998 A CN 2013102771998A CN 201310277199 A CN201310277199 A CN 201310277199A CN 103305580 A CN103305580 A CN 103305580A
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Abstract
The invention discloses a method for preparing collagen peptide from mammal skin and bone. The method comprises the steps of raw material pretreatment, degreasing in a degreasing machine, enzymolysis through bio-enzyme A and bio-enzyme B, and oil-liquid separation, specifically comprises the steps of reserving clear liquor on the lower side, intercepting collagen peptide with molecular weight greater than 3000Da, clearing ionic impurities, sterilizing and condensing and drying, wherein the bio-enzyme A is any one or any mixtures of neutral protease, alkaline protease and trypsin; the bio-enzyme B is any one or any mixtures of strepto-collagenase, acid protease, papain and bromelain. The collagen peptide which is low in molecular weight is prepared by pure biological and physical ways, and is free from chemical treatment to raw material, or organic chemical or inorganic chemical in the preparation process; the prepared collagen peptide is relatively high in purity and safety, and good in application effect.
Description
Technical field
The present invention relates to the preparation method of collagen peptide, be specifically related to a kind of method for preparing collagen peptide take skin of mammal and bone as raw material.
Background technology
Collagen peptide was sold fiery in recent years in beauty industry, its effect is praised highly by the human consumer more and more significantly.Now, collagen peptide has been widely used in the fields such as health care, food, makeup.The application of collagen peptide aspect beauty and health care expanded to fat-reducing, chest enlarge, skin makeup, strong bone, anti-ageing, improve sleep quality and body immunity.Moreover, collagen peptide also is applied in the improvement, some senile disease of the elderly, as replenishes the calcium, consolidates calcium etc.
Most collagen peptides adopt chemical process to make with fish raw material (fish-skin, fish scale, the flesh of fish or fish viscera) on the existing market, in preparation process, need to add inorganic chemical, organic chemicals, such as sodium bicarbonate, sodium-chlor, grease-removing agent, tensio-active agent etc.The technique that chemical process prepares collagen peptide is numerous and diverse loaded down with trivial details, in preparation process, can make finished product mix band impurity, and some chemicals can make the amino acid group sex change of collagen peptide, thereby affected the performance of product, efficient when having reduced product application, and bring latent property potential safety hazard when using.In addition, from biological angle, the similarity of the molecular structure of the molecular structure of the collagen protein of fish and the collagen protein of human body is far below the similarity of the molecular structure of the collagen protein of the molecular structure of mammiferous collagen protein and human body.For example: the similarity of the molecular structure of the molecular structure of porcine collagen and the collagen protein of human body reaches more than 90%, aminoacid sequence on the molecular chain is arranged and amino acid kind quantity and human body almost consistent, biological homology of this explanation pig and people is very high, the collagen peptide for preparing take pig as raw material to the beauty and health care effect of human body also can be better, security is also higher.
Summary of the invention
The object of the invention is to provide a kind of method for preparing collagen peptide to feed thing animal skin and bone as raw material, the method adopts the mode of pure biology, physics to obtain low-molecular-weight collagen peptide, in preparation process, raw material is not carried out chemical treatment, do not add organic chemicals, inorganic chemical, that the collagen peptide purity of acquisition and safety are given birth to is higher, effect good.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method for preparing collagen peptide take skin of mammal and bone as raw material is characterized in that may further comprise the steps:
1) raw materials pretreatment;
2) in degreasing machine, carry out degreasing;
3) adopt biological enzyme A and biological enzyme B to carry out enzymolysis;
4) fluid separates, and gets clear liquor;
5) the amputation molecular weight is the above collagen peptide of 3000Da;
6) remove type impurity ion;
7) sterilization;
8) concentrated;
9) drying;
Described biological enzyme A is one or more mixing in neutral protease, Sumizyme MP, the trypsinase; Described biological enzyme B is one or more mixing in hammer collagenase, aspartic protease, papain, the Traumanase.
Step 1) is placed on raw material in the rinse bath and cleans with normal-temperature water, then is cut into the fritter that length is 1～10cm.
Step 2) raw material is placed 60～100 ℃ of hot water pump into the degreasing machine degreasing under stirring.
Step 3) adds purified water first in raw material, then be warming up to 45～50 ℃, 0.2～1% the biological enzyme A enzymolysis 2～4 hours that adds raw material weight adds 0.1～1% the biological enzyme B enzymolysis 3～5 hours of raw material weight again, is warming up at last 85～90 ℃ and be incubated 30～60 minutes.Biological enzyme A and biological enzyme carry out enzymolysis for the not isoschizomer of collagen protein respectively, carry out enzymolysis with biological enzyme A first, yet carry out enzymolysis with biological enzyme B again, can overcome the defective that collagen peptide molecular weight that two kinds of enzymes produce during enzymolysis simultaneously is lower than 300Da, under the processing parameter condition of regulation, the molecular weight of the collagen peptide of enzymolysis gained mostly concentrates between 500～1500Da, and security and the purity of product are high, and effect is good.
Decolour with activity charcoal powder first behind the step 3) enzymolysis, carry out fluid again and separate, the consumption of gac is preferably 3～25% of raw material weight.
Step 4) is carried out fluid with whizzer and is separated; Step 5) ultrafiltration post amputation small molecules collagen peptide; Step 6) adopts deionization apparatus to remove ionic impurity, and described deionization apparatus is that one or more series connection in chromatography column, ion exchange column, reverse osmosis membrane, electroosmosis board or the electro-adsorption device are used, to remove the negatively charged ion of heavy metal ion and trace.
Step 7) adopts the constant temperature Sterilizers to sterilize, and the temperature of sterilization is 85～95 ℃, and the time is 30～60 minutes.
Remove with the flat sheet membrane strainer first after the step 7) sterilization and degerm, carry out drying again, the aperture of the flat sheet membrane in the flat sheet membrane strainer is preferably 0.1～0.5 μ m.
Step 8) adopts the vacuum flashing vaporizer to carry out cryoconcentration, and vacuum tightness is 10～100Pa, vaporization temperature≤40 ℃, and steam output is 200～1500kg/h.
In step 9) employing freeze drier, spray-drier, the Vacuumdrier one or both carry out drying.
Compared with prior art, the invention has the beneficial effects as follows:
1, technique of the present invention is simple, and easily operation utilizes existing equipment and biological enzyme formulation to implement;
2, the present invention's processing that raw material is carried out is the combination of biological mode and physics mode, the Physical Processing mode all adopts existing mechanical means that raw material is carried out physical treatment, do not add any chemical reagent, make finished product not mix band impurity, and can keep the collagen peptide unchangeability; The biological processing mode is to adopt existing biological enzyme, by the controlled working condition, has obtained to have divided and has measured moderate collagen peptide, and the combination of biological mode and physics mode can improve purity and the performance of product, greatly improves the effect of product;
3, the present invention is take skin of mammal and bone as raw material, the similarity of the molecular structure of the molecular structure of its collagen protein and the collagen protein of human body is high, the low-molecular weight collagen peptide that obtains is safe, the efficient height of application, finished product is suitable for also being suitable in the various makeup in the product such as the healthcare products, nutritious supplementary, seasonings of class for oral administration.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below by the implementation example the present invention is further described in detail.
A kind of method for preparing collagen peptide take skin of mammal and bone as raw material is characterized in that may further comprise the steps in turn:
1) raw materials pretreatment: take mammiferous skin or bone as raw material, such as pigskin, ox-hide, sheepskin, pig bone, sheep bone etc. puts into rinse bath with raw material to clean up, and then being cut into length is the long fritter of 1～10cm;
2) raw material is placed the stock chest of having put 60～100 ℃ of hot water, pumps into degreasing in the degreasing machine under stirring;
3) raw material after the degreasing adds first purified water, then be warming up to 45～50 ℃, 0.2～1% the biological enzyme A enzymolysis 2～4 hours that adds raw material weight, 0.1～1% the biological enzyme B enzymolysis 3～5 hours that adds again raw material weight, be warming up at last 85～90 ℃ and be incubated 30～60 minutes, described biological enzyme A is one or more mixing in neutral protease, Sumizyme MP, the trypsinase, and described biological enzyme B is one or more mixing in hammer collagenase, aspartic protease, papain, the Traumanase;
4) leave standstill 0.5～1 hour behind the enzymolysis, make the suspending sundries and the grease that produce behind the enzymolysis place the upper strata, the liquid discharge will be left standstill in the bottom of slave unit, obtain collagen peptide liquid;
5) 3～25% of the adding raw material weight gac stirs 30～50min and decolours under 60～90 ℃ of temperature, with filter gac is removed, and obtains the collagen peptide liquid of transparent cleaning;
6) separate carrying out fluid in the collagen peptide liquid input whizzer, again slough grease;
7) the collagen peptide liquid that step 6) is obtained drops in the ultrafiltration post, and the amputation molecular weight is the above collagen peptide of 3000Da;
8) adopt deionization apparatus to remove ionic impurity, described deionization apparatus can use for one or more series connection in chromatography column, ion exchange column, reverse osmosis membrane, electroosmosis board or the electro-adsorption device, removes the negatively charged ion of heavy metal ion and trace;
9) sterilization: adopt the constant temperature Sterilizers to sterilize, temperature is 85～95 ℃, and the time is 30～60 minutes;
10) rear the removing with the flat sheet membrane strainer of sterilization degermed, and the thickness of the flat sheet membrane in the flat sheet membrane strainer is preferably 0.1～0.5 μ m;
11) adopt the vacuum flashing vaporizer to carry out cryoconcentration, vacuum tightness is 10～100Pa, vaporization temperature≤30 ℃, and steam output is 200～1500kg/h;
12) one or both in employing freeze drier, spray-drier, the Vacuumdrier carry out drying, obtain the collagen peptide of powder-type.
Embodiment 1
Get pigskin 200kg, in rinse bath, clean 3 times under the normal temperature, add water 800kg, dynamic cleaning 30min at every turn.Peace and quiet pigskin is cut into the little skin bit that length is 1～10cm with dermatome.The little skin bit that cuts is placed stock chest, add 90 ℃ of hot water, pump into degreasing in the degreasing machine under stirring.Little skin bit after the degreasing is delivered in the stainless steel cauldron, adds the 600kg purified water, is warming up to 48 ℃, adds 1kg biological enzyme A, and enzymolysis is 3 hours under the continuously stirring, and described biological enzyme A is that neutral protease and Sumizyme MP mix.Behind the biological enzyme A enzymolysis, add 0.6kg biological enzyme B, described biological enzyme B is that hammer collagenase and sour raw albumen enzyme mix again, and enzymolysis is 4 hours under the continuously stirring, and degree of hydrolysis has reached 92%, is warmed up to 90 ℃, insulation 40min.After leaving standstill 1 hour, the slave unit bottom emits clear liquor.In clear liquor, add the 10kg gac, under 80 ℃ of temperature, stir decolouring 40min, with filter gac is removed, obtain the collagen peptide liquid of transparent cleaning.Collagen peptide liquid pump after the decolouring is entered to carry out in the whizzer fluid separate, obtain lipid content and be lower than 1% qualified collagen peptide liquid.The collagen peptide liquid pump is entered in the ultrafiltration post, the amputation molecular weight obtains low-molecular-weight collagen peptide liquid greater than the molecule of 3000Da again.The collagen peptide liquid pump is entered in chromatography column and the electro-adsorption device series component, and heavy-metal ion removal and negatively charged ion obtain pure collagen peptide liquid.Pure collagen peptide liquid pump is entered in the constant temperature Sterilizers, and 90 ℃ of sterilization 45min remove a large amount of bacteriums.Collagen peptide liquid pump after the sterilization is entered to carry out cryoconcentration in the vacuum flashing vaporizer, and the vacuum tightness of equipment is 50Pa, and vaporization temperature is 28 ℃, and steam output is 800kg/h, and the cryoconcentration time is 45min.Concentrated solution pumped in the flat sheet membrane strainer bacterium is removed, the aperture of flat sheet membrane is 0.15 μ m.At last concentrated solution is pumped into drying in the spray-drier, obtain flaxen collagen protein Gly-His-Lys, the smell of product is pure.
Embodiment 2
Get ox-hide 200kg, in rinse bath, clean 3 times under the normal temperature, add water 800kg, dynamic cleaning 30min at every turn.Peace and quiet pigskin is cut into the little skin bit that length is 1～10cm with dermatome.The little skin bit that cuts is placed stock chest, add 100 ℃ of hot water, pump into degreasing in the degreasing machine under stirring.Little skin bit after the degreasing is delivered in the stainless steel cauldron, adds the 600kg purified water, is warming up to 45 ℃, adds 0.6kg trypsinase, and enzymolysis is 4 hours under the continuously stirring.Behind the trypsin digestion, add 1kg biological enzyme B, described biological enzyme B is that papain and Traumanase mix again, and enzymolysis is 3 hours under the continuously stirring, and degree of hydrolysis has reached 92%, is warmed up to 85 ℃, insulation 30min.After leaving standstill 1 hour, the slave unit bottom emits clear liquor.In clear liquor, add the 6kg gac, under 60 ℃ of temperature, stir decolouring 50min, with filter gac is removed, obtain the collagen peptide liquid of transparent cleaning.Collagen peptide liquid pump after the decolouring is entered to carry out in the whizzer fluid separate, obtain lipid content and be lower than 1% qualified collagen peptide liquid.The collagen peptide liquid pump is entered in the ultrafiltration post, the amputation molecular weight obtains low-molecular-weight collagen peptide liquid greater than the molecule of 3000Da again.The collagen peptide liquid pump is entered in the ion exchange column, and heavy-metal ion removal and negatively charged ion obtain pure collagen peptide liquid.Pure collagen peptide liquid pump is entered in the constant temperature Sterilizers, and 95 ℃ of sterilization 30min remove a large amount of bacteriums.Collagen peptide liquid pump after the sterilization is entered to carry out cryoconcentration in the vacuum flashing vaporizer, and the vacuum tightness in the equipment is 100Pa, and vaporization temperature is 32 ℃, and steam output is 1000kg/h, and the cryoconcentration time is 35min.Concentrated solution pumped in the flat sheet membrane strainer bacterium is removed, the aperture of flat sheet membrane is 0.15 μ m.At last concentrated solution is pumped into drying in the Vacuumdrier, obtain flaxen collagen protein Gly-His-Lys, the smell of product is pure.
Embodiment 3
Get sheep bone 200kg, in rinse bath, clean 3 times under the normal temperature, add water 800kg, dynamic cleaning 30min at every turn.Peace and quiet sheep bone machine is cut into the ossiculum piece that length is 1～10cm.The ossiculum piece that cuts is placed stock chest, add 80 ℃ of hot water, pump into degreasing in the degreasing machine under stirring.Ossiculum piece after the degreasing is delivered in the stainless steel cauldron, adds the 600kg purified water, is warming up to 50 ℃, adds 2kg biological enzyme A, and described biological enzyme A is neutral protease, Sumizyme MP, trypsinase three mixing, and enzymolysis is 3 hours under the continuously stirring.Behind the biological enzyme A enzymolysis, add 1kg hammer collagenase, enzymolysis is 4 hours under the continuously stirring again, and degree of hydrolysis has reached 95%, is warmed up to 90 ℃, insulation 40min.After leaving standstill 1 hour, the slave unit bottom emits clear liquor.In clear liquor, add the 40kg gac, under 80 ℃ of temperature, stir decolouring 30min, with filter gac is removed, obtain the collagen peptide liquid of transparent cleaning.Collagen peptide liquid pump after the decolouring is entered to carry out in the whizzer fluid separate, obtain lipid content and be lower than 1% qualified collagen peptide liquid.The collagen peptide liquid pump is entered in the ultrafiltration post, the amputation molecular weight obtains low-molecular-weight collagen peptide liquid greater than the molecule of 3000Da again.The collagen peptide liquid pump is entered in the reverse osmosis membrane, and heavy-metal ion removal and negatively charged ion obtain pure collagen peptide liquid.Pure collagen peptide liquid pump is entered in the constant temperature Sterilizers, and 85 ℃ of sterilization 60min remove a large amount of bacteriums.Collagen peptide liquid pump after the sterilization is entered to carry out cryoconcentration in the vacuum flashing vaporizer, and the vacuum tightness in the equipment is 10Pa, and vaporization temperature is 40 ℃, and steam output is 200kg/h, and the cryoconcentration time is 40min.Concentrated solution pumped in the flat sheet membrane strainer bacterium is removed, the aperture of flat sheet membrane is 0.1 μ m.At last concentrated solution is pumped into drying in the freeze drier, obtain flaxen collagen protein Gly-His-Lys, the smell of product is pure.
The according to the above description announcement of book and instruction, those skilled in the art in the invention can also change and revise above-mentioned embodiment.Therefore, the embodiment that discloses and describe above the present invention is not limited to also should fall in the protection domain of claim of the present invention modifications and changes more of the present invention.In addition, although used some specific terms in this specification sheets, these terms do not consist of any restriction to the present invention just for convenience of description.
Claims (10)
1. method for preparing collagen peptide take skin of mammal and bone as raw material is characterized in that may further comprise the steps at least:
1) raw materials pretreatment;
2) in degreasing machine, carry out degreasing;
3) biological enzyme A and biological enzyme B carry out enzymolysis;
4) fluid separates, and gets clear liquor;
5) the amputation molecular weight is the above collagen peptide of 3000Da;
6) remove type impurity ion;
7) sterilization;
8) concentrated;
9) drying;
Described biological enzyme A is one or more mixing in neutral protease, Sumizyme MP, the trypsinase; Described biological enzyme B is one or more mixing in hammer collagenase, aspartic protease, papain, the Traumanase.
2. the method for preparing collagen peptide take skin of mammal and bone as raw material as claimed in claim 1, it is characterized in that: step 1) is cleaned raw material and stripping and slicing.
3. the method for preparing collagen peptide take skin of mammal and bone as raw material as claimed in claim 1 is characterized in that: step 2) place 60～100 ℃ of hot water to pump into degreasing machine under stirring raw material to carry out degreasing.
4. the method for preparing collagen peptide take skin of mammal and bone as raw material as claimed in claim 1, it is characterized in that: step 3) adds purified water first in raw material, then be warming up to 45～50 ℃, 0.2～1% the biological enzyme A enzymolysis 2～4 hours that adds raw material weight, 0.1～1% the biological enzyme B enzymolysis 3～5 hours that adds again raw material weight is warming up to 85～90 ℃ and be incubated 30～40 minutes at last.
5. the method for preparing collagen peptide take skin of mammal and bone as raw material as claimed in claim 1 is characterized in that: decolour with activity charcoal powder first behind the step 3) enzymolysis, carry out fluid again and separate.
6. the method for preparing collagen peptide take skin of mammal and bone as raw material as claimed in claim 1, it is characterized in that: step 4) is carried out fluid with whizzer and is separated, step 5) is the above collagen peptide of 3000Da with ultrafiltration post amputation molecular weight, step 6) adopts deionization apparatus to remove ionic impurity, and described deionization apparatus is that one or more series connection in chromatography column, ion exchange column, reverse osmosis membrane, electroosmosis board or the electro-adsorption device are used.
7. the method for preparing collagen peptide take skin of mammal and bone as raw material as claimed in claim 1, it is characterized in that: step 7) adopts the constant temperature Sterilizers to sterilize, and the temperature of sterilization is 85～95 ℃, and the time is 30～60 minutes.
8. the method for preparing collagen peptide take skin of mammal and bone as raw material as claimed in claim 1 is characterized in that: remove with the flat sheet membrane strainer first after the step 7) sterilization and degerm, carry out drying again.
9. the method for preparing collagen peptide take skin of mammal and bone as raw material as claimed in claim 1, it is characterized in that: step 8) adopts the vacuum flashing vaporizer to carry out cryoconcentration, vacuum tightness is 10～100Pa, vaporization temperature≤40 ℃, and steam output is 200～1500kg/h.
10. the method for preparing collagen peptide take skin of mammal and bone as raw material as claimed in claim 1 is characterized in that: step 9) adopts in freeze drier, spray-drier, the Vacuumdrier one or both to carry out drying.
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Cited By (10)
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| CN103920173A (en) * | 2014-04-10 | 2014-07-16 | 广州康洛信生物科技有限公司 | Collagen safe sterilizing method |
| CN104398399A (en) * | 2014-11-14 | 2015-03-11 | 唯美度科技（北京）有限公司 | Composite glycopeptide breast beauty cream and preparation method thereof |
| CN104606668A (en) * | 2015-02-06 | 2015-05-13 | 深圳唯美度生物科技有限公司 | Breast enlargement gel containing complex polypeptides and process thereof |
| CN104814500A (en) * | 2015-04-17 | 2015-08-05 | 马文浩 | Aesthetic health care beverages for strengthening the bones and muscles and skin and a preparation method thereof |
| CN104830937A (en) * | 2015-05-14 | 2015-08-12 | 吉林大学 | Method for preparing peptone by using chicken slaughtering by-products |
| CN105831734A (en) * | 2016-03-25 | 2016-08-10 | 中国农业科学院农产品加工研究所 | Method of gradient in-series membrane concentration for bone extract liquid |
| CN107142294A (en) * | 2017-06-16 | 2017-09-08 | 吉林省东鳌鹿业集团有限公司 | The method that collagen peptides products are prepared by raw material of deerskin |
| CN108925742A (en) * | 2018-05-25 | 2018-12-04 | 余碧芝 | Bone collagen peptide and its production method with gel characteristic |
| CN109321624A (en) * | 2018-11-15 | 2019-02-12 | 安徽嘉润生物科技有限责任公司 | A kind of enzymolysis process of fresh porcine skin preparation active collagen peptide |
| CN109457006A (en) * | 2018-11-26 | 2019-03-12 | 天津市天大天福生物技术有限公司 | A kind of convenient preparation method of the gradient peptide of different molecular weight mixing |
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| CN103920173A (en) * | 2014-04-10 | 2014-07-16 | 广州康洛信生物科技有限公司 | Collagen safe sterilizing method |
| CN103920173B (en) * | 2014-04-10 | 2016-11-02 | 广州康洛信生物科技有限公司 | Collagen protein safe sterilization method |
| CN104398399A (en) * | 2014-11-14 | 2015-03-11 | 唯美度科技（北京）有限公司 | Composite glycopeptide breast beauty cream and preparation method thereof |
| CN104606668A (en) * | 2015-02-06 | 2015-05-13 | 深圳唯美度生物科技有限公司 | Breast enlargement gel containing complex polypeptides and process thereof |
| CN104814500A (en) * | 2015-04-17 | 2015-08-05 | 马文浩 | Aesthetic health care beverages for strengthening the bones and muscles and skin and a preparation method thereof |
| CN104830937A (en) * | 2015-05-14 | 2015-08-12 | 吉林大学 | Method for preparing peptone by using chicken slaughtering by-products |
| CN105831734A (en) * | 2016-03-25 | 2016-08-10 | 中国农业科学院农产品加工研究所 | Method of gradient in-series membrane concentration for bone extract liquid |
| CN105831734B (en) * | 2016-03-25 | 2020-03-10 | 中国农业科学院农产品加工研究所 | Method for concentrating bone extract by gradient series membrane |
| CN107142294A (en) * | 2017-06-16 | 2017-09-08 | 吉林省东鳌鹿业集团有限公司 | The method that collagen peptides products are prepared by raw material of deerskin |
| CN108925742A (en) * | 2018-05-25 | 2018-12-04 | 余碧芝 | Bone collagen peptide and its production method with gel characteristic |
| CN109321624A (en) * | 2018-11-15 | 2019-02-12 | 安徽嘉润生物科技有限责任公司 | A kind of enzymolysis process of fresh porcine skin preparation active collagen peptide |
| CN109457006A (en) * | 2018-11-26 | 2019-03-12 | 天津市天大天福生物技术有限公司 | A kind of convenient preparation method of the gradient peptide of different molecular weight mixing |
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Application publication date: 20130918 |