CN104587467A - ICG-encapsulated polymer-phospholipid nano-particles and preparation method thereof - Google Patents
ICG-encapsulated polymer-phospholipid nano-particles and preparation method thereof Download PDFInfo
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- CN104587467A CN104587467A CN201410837172.4A CN201410837172A CN104587467A CN 104587467 A CN104587467 A CN 104587467A CN 201410837172 A CN201410837172 A CN 201410837172A CN 104587467 A CN104587467 A CN 104587467A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/24—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing atoms other than carbon, hydrogen, oxygen, halogen, nitrogen or sulfur, e.g. cyclomethicone or phospholipids
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/34—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyesters, polyamino acids, polysiloxanes, polyphosphazines, copolymers of polyalkylene glycol or poloxamers
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Abstract
The invention provides an ICG-encapsulated polymer-phospholipid nanoparticle, which comprises an inner core and an outer shell, wherein the inner core is formed by coating a polymer on the surface of the ICG, the outer shell is phospholipid, the phospholipid is coated on the surface of the polymer, the polymer is polyglycolide-lactide or polylactic acid, and the ICG-encapsulated polymer-phospholipid nanoparticle is uniform in particle size and stable in property. The invention also provides a preparation method of the ICG-encapsulated polymer-phospholipid nanoparticles, the ICG-encapsulated polymer-phospholipid nanoparticles are prepared by adopting a one-step high-pressure homogenizing method, the preparation method is simple, and a large amount of ICG-encapsulated polymer-phospholipid nanoparticles can be prepared.
Description
Technical field
The present invention relates to pharmaceutical carrier field, be specifically related to a kind of bag and carry polymer-phospholipid nano-particle of ICG and preparation method thereof.
Background technology
Polymer nano granules and nanometer liposome are that two class main flow nano-carriers of representative can efficiently wrap up and transmit medicine or gene etc., become the study hotspot of various countries scientist.Polymer nano granules has the advantages such as drug encapsulation ability is strong, cell endocytic efficiency is high, circulation time in vivo is long.Nanometer liposome possesses the characteristics such as biological safety is excellent, transmittability is efficient, preparation technology is simple.The polymer-phospholipid nano-particle that conjugated polymer and phospholipid advantage is separately prepared has been widely used in the transmission of medicine.But existing polymer-phospholipid nanometer grain preparation method is mainly ultrasonic method and nanometer precipitation method, the dosage of preparation is confined to the test dose of 1-3 milliliter, limits the industrialization process of polymer-phospholipid nano-particle.
Summary of the invention
For solving the problem, the invention provides a kind of bag and carrying polymer-phospholipid nano-particle of ICG and preparation method thereof.The polymer-phospholipid nano-particle that bag of the present invention carries ICG adopts a step high-pressure homogenization preparation, preparation method is simple, heavy dose of polymer-phospholipid nano-particle can be prepared, solve polymer-phospholipid nano-particle in prior art and prepare the less problem of dosage.
First aspect present invention provides the polymer-phospholipid nano-particle that a kind of bag carries ICG (indocyanine green), the polymer-phospholipid nano-particle that described bag carries ICG comprises kernel and shell, described kernel is formed on ICG surface by polymer overmold, described shell is phospholipid, described phospholipid is coated on described polymer surfaces, and described polymer is poly (glycolide-co-lactide) (PLGA) or polylactic acid (PLA).
Preferably, described phospholipid is at least one in soybean lecithin, hydrogenated soy phosphatidyl choline, Ovum Gallus domesticus Flavus lecithin, hydrogenated yolk lecithin, phosphatidylcholine and PHOSPHATIDYL ETHANOLAMINE.
Preferably, the mass ratio of described polymer and described ICG is 1:0.8-2.4, and the mass ratio of described phospholipid and described ICG is 1:1-3.
Preferably, described bag carries the particle diameter of the polymer-phospholipid nano-particle of ICG is 20-300nm.
The bag that first aspect present invention provides carries that the polymer-phospholipid nano particle diameter of ICG is homogeneous, stable in properties, place and not occur sedimentation, solidifying wadding phenomenon after 30 days, the polymer-phospholipid nano-particle that described bag carries ICG can be used for targets identification and the photo-thermal therapy of tumor.
Second aspect present invention provides the preparation method that a kind of bag carries the polymer-phospholipid nano-particle of ICG, comprises the following steps:
(1) be dissolved in solvent by phospholipid and ICG, obtain mixed solution, at 60 DEG C-90 DEG C, pressure is under 500-1400bar condition, described mixed solution is carried out primary emulsifying 1-5min, obtains emulsion;
(2) in described emulsion, polymer solution is dripped, at 60 DEG C-90 DEG C, pressure is under 500-1400bar condition, continue emulsifying 4-6min, form the solution of the polymer-phospholipid nano-particle carrying ICG containing bag, obtain the described polymer-phospholipid nano-particle carrying ICG containing bag, the polymer-phospholipid nano-particle that described bag carries ICG comprises kernel and shell, described kernel is formed on ICG surface by polymer overmold, described shell is phospholipid, described phospholipid is coated on described polymer surfaces, described polymer is poly (glycolide-co-lactide) (PLGA) or polylactic acid (PLA).
Preferably, described phospholipid is at least one in soybean lecithin, hydrogenated soy phosphatidyl choline, Ovum Gallus domesticus Flavus lecithin, hydrogenated yolk lecithin, phosphatidylcholine, PHOSPHATIDYL ETHANOLAMINE.
Preferably, the mass ratio of described polymer and described ICG is 1:0.8-2.4.
Preferably, the mass ratio of described phospholipid and described ICG is 1:1-3.
Preferably, described solvent to be mass concentration be 4% ethanol water.
Preferably, in described mixed solution, the concentration of described phospholipid is 0.15-0.75mg/mL, and the concentration of described ICG is 0.2-1.5mg/mL.
Preferably, the molecular weight of described polymer is 5000-15000.
Preferably, described dissolution of polymer is obtained described polymer solution in second cyanogen or acetone.
Preferably, the concentration of described polymer solution is 1-5mg/mL.
Preferably, the described volume carrying the solution of the polymer-phospholipid nano-particle of ICG containing bag is 50mL-1000mL.
Preferably, described bag carries the particle diameter of the polymer-phospholipid nano-particle of ICG is 20-300nm.
A kind of bag that second aspect present invention provides carries the polymer-phospholipid nanometer grain preparation method of ICG, a step high-pressure homogenization preparation bag is adopted to carry the polymer-phospholipid nano-particle of ICG, simple to operate, the polymer-phospholipid nano-particle that heavy dose of bag carries ICG can be prepared, for the amplification production of this nano-particle and clinical research provide basis, the nano particle diameter of preparation is homogeneous, stable in properties.
To sum up, the beneficial effect that a kind of bag provided by the invention carries the polymer-phospholipid nano-particle of ICG and preparation method thereof comprises the following aspects:
1, a step high-pressure homogenization provided by the invention can prepare the polymer-phospholipid nano-particle that heavy dose of bag carries ICG, for the amplification production of this nano-particle and clinical research provide basis.This preparation method is simple and easy to do, and convenient operation is promoted.
2, to carry the polymer-phospholipid nano particle diameter of ICG homogeneous for described bag, and stable in properties, places after 30 days and do not occur sedimentation, solidifying wadding phenomenon.
Accompanying drawing explanation
Fig. 1 is the preparation process schematic diagram that embodiment 1 wraps the polymer-phospholipid nano-particle carrying ICG.
Detailed description of the invention
The following stated is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Embodiment 1:
Bag carries a preparation method for the polymer-phospholipid nano-particle of ICG, comprises the following steps:
(1) soybean lecithin and ICG being dissolved in mass concentration is obtain mixed solution in the ethanol water of 4%, and in mixed solution, the concentration of soybean lecithin is 0.15mg/mL, ICG concentration is 0.2mg/mL, and cumulative volume is 40mL; Under mixed solution being kept 90 DEG C of temperature, pressure is adjusted to 500bar, and primary emulsifying 2min, obtains emulsion;
(2) by molecular weight be 5000 polymer P LGA be dissolved in second cyanogen, obtain the PLGA solution that concentration is 1mg/mL, cumulative volume is 10mL; Drip PLGA solution in emulsion, temperature keeps 90 DEG C, and pressure keeps 500bar, continues emulsifying 4min, forms 50mL and contains the solution that bag carries the PLGA-phospholipid nano-particle of ICG, must wrap the PLGA-phospholipid nano-particle carrying ICG.
Fig. 1 is the preparation process schematic diagram that embodiment 1 wraps the polymer-phospholipid nano-particle carrying ICG, as can be seen from Figure 1, carry out primary emulsifying after soybean lecithin 1 and ICG 2 are mixed, then add polymer 3 and continue emulsifying, obtain wrapping the PLGA-phospholipid nano-particle 4 carrying ICG, the polymer-phospholipid nano-particle that this bag carries ICG comprises kernel and shell, and kernel is coated on ICG 2 surface by polymer 3 and is formed, shell is phosphatidase 1, and soybean lecithin 1 is coated on polymer 3 surface.
Be 20-300nm by particle size analyzer determination nano particle diameter.This is contained the solution of PLGA-phospholipid nano-particle that bag carries ICG and place 30 days, after 30 days, do not occur sedimentation, solidifying wadding phenomenon, illustrate that the bag with nucleocapsid structure carries the PLGA-phospholipid nano-particle character of ICG comparatively stable.
Embodiment 2:
Bag carries a preparation method for the polymer-phospholipid nano-particle of ICG, comprises the following steps:
(1) soybean lecithin and ICG being dissolved in mass concentration is obtain mixed solution in the ethanol water of 4%, and in mixed solution, the concentration range of soybean lecithin is 0.75mg/mL, ICG concentration is 1.5mg/mL, and cumulative volume is 40mL; Under mixed solution being kept 60 DEG C of temperature, pressure is adjusted to 1400bar, and primary emulsifying 2min, obtains emulsion;
(2) by molecular weight be 15000 polymer P LGA be dissolved in second cyanogen, obtain the PLGA solution that concentration is 5mg/mL, cumulative volume is 10mL; Drip PLGA solution in emulsion, temperature keeps 60 DEG C, and pressure keeps 1400bar, continues emulsifying 6min, forms 50mL and contains the solution that bag carries the PLGA-phospholipid nano-particle of ICG, must wrap the PLGA-phospholipid nano-particle carrying ICG.Be 20-300nm by particle size analyzer determination grain diameter.The polymer-phospholipid nano-particle that this bag carries ICG comprises kernel and shell, and kernel is coated on ICG surface by polymer P LGA and is formed, and shell is soybean lecithin, and soybean lecithin is coated on polymer surfaces.
Embodiment 3:
Bag carries a preparation method for the polymer-phospholipid nano-particle of ICG, comprises the following steps:
(1) soybean lecithin and ICG being dissolved in mass concentration is obtain mixed solution in the ethanol water of 4%, and in mixed solution, the concentration of soybean lecithin is 0.15mg/mL, ICG concentration is 0.2mg/mL, and cumulative volume is 800mL; Under mixed solution being kept 80 DEG C of temperature, pressure is adjusted to 500bar, and primary emulsifying 2min, obtains emulsion;
(2) by molecular weight be 10000 polymer P LGA be dissolved in second cyanogen, obtain the PLGA solution that concentration is 1mg/mL, cumulative volume is 200mL; Drip PLGA solution in emulsion, temperature keeps 80 DEG C, and pressure keeps 500bar, continues emulsifying 4min, forms 1000mL and contains the solution that bag carries the PLGA-phospholipid nano-particle of ICG, must wrap the PLGA-phospholipid nano-particle carrying ICG.Be 20-300nm by particle size analyzer determination grain diameter.The polymer-phospholipid nano-particle that this bag carries ICG comprises kernel and shell, and kernel is coated on ICG surface by polymer P LGA and is formed, and shell is soybean lecithin, and soybean lecithin is coated on polymer surfaces.
Embodiment 4:
Bag carries a preparation method for the polymer-phospholipid nano-particle of ICG, comprises the following steps:
(1) soybean lecithin and ICG being dissolved in mass concentration is obtain mixed solution in 4% ethanol water, and in mixed solution, the concentration of soybean lecithin is 0.75mg/mL, ICG concentration is 1.5mg/mL, and cumulative volume is 800mL; Under mixed solution being kept 90 DEG C of temperature, pressure is adjusted to 1400bar, primary emulsifying 1min; Obtain emulsion;
(2) by molecular weight be 15000 polymer P LGA be dissolved in second cyanogen, obtain the PLGA solution that concentration is 5mg/ml, cumulative volume is 200mL; Drip PLGA solution in emulsion, temperature keeps 90 DEG C, and pressure keeps 1400bar, continues emulsifying 6min, forms 1000mL and contains the solution that bag carries the PLGA-phospholipid nano-particle of ICG, must wrap the PLGA-phospholipid nano-particle carrying ICG.Be 20-300nm by particle size analyzer determination grain diameter.The polymer-phospholipid nano-particle that this bag carries ICG comprises kernel and shell, and kernel is coated on ICG surface by polymer P LGA and is formed, and shell is soybean lecithin, and soybean lecithin is coated on polymer surfaces.
Embodiment 5:
Bag carries a preparation method for the polymer-phospholipid nano-particle of ICG, comprises the following steps:
(1) soybean lecithin and ICG being dissolved in mass concentration is obtain mixed solution in 4% ethanol water, and in mixed solution, the concentration of soybean lecithin is 0.5mg/mL, ICG concentration is 1.5mg/mL, and cumulative volume is 800mL; Under mixed solution being kept 60 DEG C of temperature, pressure is adjusted to 800bar, and primary emulsifying 5min, obtains emulsion;
(2) by molecular weight be 15000 polymer P LGA be dissolved in second cyanogen, obtain the PLGA solution that concentration is 2.5mg/mL, cumulative volume is 200mL; Drip PLGA solution in emulsion, temperature keeps 60 DEG C, and pressure keeps 800bar, continues emulsifying 4min, forms 1000mL and contains the PLGA-phospholipid nano-particle that bag carries ICG, must wrap the PLGA-phospholipid nano-particle carrying ICG.Be 20-300nm by particle size analyzer determination grain diameter.The polymer-phospholipid nano-particle that this bag carries ICG comprises kernel and shell, and kernel is coated on ICG surface by polymer P LGA and is formed, and shell is soybean lecithin, and soybean lecithin is coated on polymer surfaces.
Embodiment 6:
Bag carries a preparation method for the polymer-phospholipid nano-particle of ICG, comprises the following steps:
(1) soybean lecithin and ICG being dissolved in mass concentration is obtain mixed solution in 4% ethanol water, and in mixed solution, the concentration of soybean lecithin is 0.5mg/mL, ICG concentration is 1.5mg/mL, and cumulative volume is 40mL; Under mixed solution being kept 90 DEG C of temperature, pressure is adjusted to 800bar, primary emulsifying 2min; Obtain emulsion;
(2) by molecular weight be 15000 polymer P LA be dissolved in second cyanogen, obtain the PLA solution that concentration is 2.5mg/mL, cumulative volume is 10mL; Drip in PLA solution to primary emulsifying liquid, temperature keeps 90 DEG C, and pressure keeps 800bar, continues emulsifying 6min, forms the solution carrying the PLA-phospholipid nano-particle of ICG containing bag of 50mL, must wrap the PLA-phospholipid nano-particle carrying ICG.Be 20-300nm by particle size analyzer determination grain diameter.The polymer-phospholipid nano-particle that this bag carries ICG comprises kernel and shell, and kernel is coated on ICG surface by polymer P LA and is formed, and shell is soybean lecithin, and soybean lecithin is coated on polymer surfaces.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. the polymer-phospholipid nano-particle of a bag year ICG, it is characterized in that, the polymer-phospholipid nano-particle that described bag carries ICG comprises kernel and shell, described kernel is formed on ICG surface by polymer overmold, described shell is phospholipid, described phospholipid is coated on described polymer surfaces, and described polymer is poly (glycolide-co-lactide) or polylactic acid.
2. nano-particle as claimed in claim 1, it is characterized in that, described phospholipid is at least one in soybean lecithin, hydrogenated soy phosphatidyl choline, Ovum Gallus domesticus Flavus lecithin, hydrogenated yolk lecithin, phosphatidylcholine and PHOSPHATIDYL ETHANOLAMINE.
3. nano-particle as claimed in claim 1, it is characterized in that, the mass ratio of described polymer and described ICG is 1:0.8-2.4, and the mass ratio of described phospholipid and described ICG is 1:1-3.
4. nano-particle as claimed in claim 1, it is characterized in that, the particle diameter that described bag carries the polymer-phospholipid nano-particle of ICG is 20-300nm.
5. bag carries a preparation method for the polymer-phospholipid nano-particle of ICG, it is characterized in that, comprises the following steps:
(1) phospholipid and ICG are dissolved in solvent, obtain mixed solution; At 60 DEG C-90 DEG C, pressure is under 500-1400bar condition, described mixed solution is carried out primary emulsifying 1-5min, obtains emulsion;
(2) in described emulsion, polymer solution is dripped, at 60 DEG C-90 DEG C, pressure is under 500-1400bar condition, continue emulsifying 4-6min, form the solution of the polymer-phospholipid nano-particle carrying ICG containing bag, obtain the described polymer-phospholipid nano-particle carrying ICG containing bag, the polymer-phospholipid nano-particle that described bag carries ICG comprises kernel and shell, described kernel is formed on ICG surface by polymer overmold, described shell is phospholipid, described phospholipid is coated on described polymer surfaces, and described polymer is poly (glycolide-co-lactide) or polylactic acid.
6. the preparation method of nano-particle as claimed in claim 5, it is characterized in that, described phospholipid is at least one in soybean lecithin, hydrogenated soy phosphatidyl choline, Ovum Gallus domesticus Flavus lecithin, hydrogenated yolk lecithin, phosphatidylcholine and PHOSPHATIDYL ETHANOLAMINE.
7. the preparation method of nano-particle as claimed in claim 5, it is characterized in that, the mass ratio of described polymer and described ICG is 1:0.8-2.4, and the mass ratio of described phospholipid and described ICG is 1:1-3.
8. the preparation method of nano-particle as claimed in claim 5, it is characterized in that, in described mixed solution, the concentration of described phospholipid is 0.15-0.75mg/mL, and the concentration of described ICG is 0.2-1.5mg/mL.
9. the preparation method of nano-particle as claimed in claim 5, it is characterized in that, the concentration of described polymer solution is 1-5mg/mL.
10. the preparation method of nano-particle as claimed in claim 5, it is characterized in that, the particle diameter that described bag carries the polymer-phospholipid nano-particle of ICG is 20-300nm.
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| CN201410837172.4A CN104587467B (en) | 2014-12-26 | 2014-12-26 | ICG-encapsulated polymer-phospholipid nano-particles and preparation method thereof |
| PCT/CN2015/098050 WO2016101854A1 (en) | 2014-12-26 | 2015-12-21 | Icg-encapsulated polymer-phospholipid nanoparticle and preparation method therefor |
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|---|---|---|---|---|
| WO2016101854A1 (en) * | 2014-12-26 | 2016-06-30 | 深圳先进技术研究院 | Icg-encapsulated polymer-phospholipid nanoparticle and preparation method therefor |
| CN118319818A (en) * | 2024-06-13 | 2024-07-12 | 天津聚立友合科技发展有限公司 | Skin nourishing nursing antibacterial agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103239729A (en) * | 2013-04-27 | 2013-08-14 | 深圳先进技术研究院 | Nano-carrier containing hyperbranched polymer and phospholipids as well as preparation method and application for same |
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| CN102533248B (en) * | 2010-12-27 | 2014-03-26 | 中国科学院深圳先进技术研究院 | Fluorescence nanometer probe and preparation method thereof |
| CN103861123A (en) * | 2012-12-17 | 2014-06-18 | 中国科学院深圳先进技术研究院 | Diagnosis-treatment integrated nanometer material, diagnosis-treatment integrated nanometer preparation and preparation method of nanometer preparation |
| CN104587467B (en) * | 2014-12-26 | 2018-02-27 | 深圳先进技术研究院 | ICG-encapsulated polymer-phospholipid nano-particles and preparation method thereof |
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| CN103239729A (en) * | 2013-04-27 | 2013-08-14 | 深圳先进技术研究院 | Nano-carrier containing hyperbranched polymer and phospholipids as well as preparation method and application for same |
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| MINGBIN ZHENG ET AL.: "Single-Step Assembly of DOX/ICG Loaded Lipid-Polymer Nanoparticles for Highly Effective Chemo-photothermal Combination Therapy", 《ACSNANO》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016101854A1 (en) * | 2014-12-26 | 2016-06-30 | 深圳先进技术研究院 | Icg-encapsulated polymer-phospholipid nanoparticle and preparation method therefor |
| CN118319818A (en) * | 2024-06-13 | 2024-07-12 | 天津聚立友合科技发展有限公司 | Skin nourishing nursing antibacterial agent and preparation method thereof |
| CN118319818B (en) * | 2024-06-13 | 2024-08-27 | 天津聚立友合科技发展有限公司 | Skin nourishing nursing antibacterial agent and preparation method thereof |
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