發(fā)布時(shí)間：2018-07-15 10:46

【摘要】：復(fù)合樹(shù)脂及其粘接系統(tǒng)因?yàn)榫哂袃?yōu)良的美學(xué)效果，以及簡(jiǎn)便的臨床操作過(guò)程等優(yōu)勢(shì)，近年來(lái)廣泛應(yīng)用于修復(fù)牙體缺損和改善牙齒外觀(guān)。但相較其他口腔修復(fù)材料，復(fù)合樹(shù)脂更容易在表面堆積菌斑生物膜，同時(shí)復(fù)合樹(shù)脂的聚合收縮和粘接不良易導(dǎo)致邊緣微滲漏，成為唾液和細(xì)菌進(jìn)出的通道，即菌斑生物膜的入侵途徑。菌斑生物膜是引起繼發(fā)齲和修復(fù)失敗的主要原因，一方面會(huì)直接引起某些口腔軟硬組織感染性疾病，，如繼發(fā)齲、義齒性口炎，另一方面則能造成材料的老化粗糙，導(dǎo)致材料性能下降，從而更易吸引細(xì)菌黏附。這樣的惡性循環(huán)最終將會(huì)造成修復(fù)失敗，甚至對(duì)全身產(chǎn)生不良影響。修復(fù)失敗的再修復(fù)所花費(fèi)的時(shí)間占到牙醫(yī)操作時(shí)間的50-70%，而全美每年再修復(fù)的花費(fèi)更是超過(guò)200億美金。正因?yàn)閺?fù)合樹(shù)脂缺乏抗菌作用，賦予復(fù)合樹(shù)脂本身，及將復(fù)合樹(shù)脂與牙體粘接起來(lái)的粘接系統(tǒng)抗菌作用，就顯得尤為必要。具有抗菌性能的復(fù)合樹(shù)脂和粘接系統(tǒng)能減小對(duì)口腔微生態(tài)環(huán)境的影響，改善修復(fù)體的長(zhǎng)期臨床效果，維護(hù)口腔微生態(tài)環(huán)境的健康。各國(guó)研究人員在研制開(kāi)發(fā)具有抗菌作用的復(fù)合樹(shù)脂和粘接系統(tǒng)等材料方面進(jìn)行了大量的研究，以期達(dá)到抑制細(xì)菌生長(zhǎng)，防止菌斑生物膜的附著，預(yù)防繼發(fā)齲的發(fā)生，防治修復(fù)失敗和因修復(fù)體引發(fā)的感染和炎癥的目的。 本課題主要從以下四個(gè)部分進(jìn)行研究： 第一部分抗菌粘接系統(tǒng)的研發(fā)和檢測(cè):季銨鹽和納米銀顆粒改性牙本質(zhì)粘接劑對(duì)粘接強(qiáng)度和牙菌斑生物膜的影響; 第二部分添加無(wú)定型磷酸鈣納米顆粒，賦予粘接劑再礦化性能：新型含納米銀和無(wú)定形磷酸鈣的牙本質(zhì)粘接劑； 第三部分烷基鏈長(zhǎng)度的影響：含有新型抗菌季銨鹽單體甲基丙烯酸十二烷基二甲銨的牙本質(zhì)粘接系統(tǒng)； 第四部分長(zhǎng)期效果：水老化對(duì)抗菌粘接系統(tǒng)的機(jī)械性能及抗菌性能影響。 第一部分季銨鹽和納米銀顆粒改性牙本質(zhì)粘接劑對(duì)粘接強(qiáng)度和牙菌斑生物膜的影響 目的：抗菌牙本質(zhì)粘接劑在抑制殘留細(xì)菌和阻止細(xì)菌入侵方面有很重要的作用。本研究的目的是開(kāi)發(fā)一種含有新型季銨鹽單體二甲基丙烯酸季銨（quaternary ammonium dimethacrylate， QADM）和納米銀顆粒（nanoparticles of silver, NAg）的抗菌牙本質(zhì)粘接劑，并對(duì)含有QADM-NAg的粘接劑及底膠對(duì)牙本質(zhì)粘接強(qiáng)度和牙菌斑生物膜的影響進(jìn)行研究。 方法：商品化的牙本質(zhì)粘接劑及底膠Scotchbond Multi-Purpose作為本實(shí)驗(yàn)的對(duì)照組。實(shí)驗(yàn)組粘接劑和底膠是在對(duì)照組中加入QADM和NAg。測(cè)試了10組人牙本質(zhì)剪切粘接強(qiáng)度（n=10）。使用人唾液培養(yǎng)所得到牙菌斑全菌生物膜模型來(lái)研究生物膜的代謝活性，菌落形成單位（colony forming unit, CFU）計(jì)數(shù)，產(chǎn)乳酸量，死/活細(xì)菌染色（n=6）。 結(jié)果：添加了QADM和NAg的牙本質(zhì)粘接劑和底膠，其牙本質(zhì)剪切粘接強(qiáng)度沒(méi)有下降，仍介于30至35兆帕間（P0.1）。掃描電子顯微鏡（scanningelectron microscope, SEM）照片顯示有大量樹(shù)脂突形成，這在對(duì)照組和添加了QADM和NAg的實(shí)驗(yàn)組中是相同的。與對(duì)照組相比，添加QADM和NAg的對(duì)照組菌斑生物膜的代謝活性顯著降低。在粘接劑里同時(shí)添加QADM和NAg比添加單一的抗菌成分具有更強(qiáng)的抗菌作用（P0.05）。與對(duì)照組相比，同時(shí)在粘接劑和底膠中添加QADM和NAg具有最強(qiáng)的抗菌活性，最大程度降低了菌斑生物膜代謝活性，減少了CFU計(jì)數(shù)和一個(gè)數(shù)量級(jí)的產(chǎn)乳酸量。 意義：在不影響牙本質(zhì)粘接強(qiáng)度和樹(shù)脂突形態(tài)的前提下，本研究第一次證實(shí)了含有QADM和NAg的牙本質(zhì)粘接劑和底膠，對(duì)牙菌斑生物膜具有較強(qiáng)的抗菌作用。含有QADM和NAg的牙本質(zhì)粘接劑和底膠在抑制窩洞中殘留細(xì)菌和阻止細(xì)菌入侵方面有很重要的作用，因此可以預(yù)防繼發(fā)齲的的發(fā)生。QADM和NAg添加到其他牙本質(zhì)粘接系統(tǒng)可能同樣具有廣泛的應(yīng)用前景。 第二部分新型含納米銀和無(wú)定形磷酸鈣的牙本質(zhì)粘接劑 目的：抗菌牙本質(zhì)粘接劑在抑制窩洞中殘留細(xì)菌和在修復(fù)體邊緣阻止細(xì)菌入侵方面發(fā)揮重要的作用。鈣（Ca）和磷酸根離子（PO4）的釋放曾被證明能夠促進(jìn)病變牙的再礦化。本研究的目標(biāo)是將納米銀顆粒NAg和無(wú)定形磷酸鈣納米顆粒（Ca3[PO4]2, nanoparticles of amorphous calcium phosphate, NACP）添加到牙本質(zhì)粘接劑中，以研究其對(duì)牙本質(zhì)粘接強(qiáng)度和牙菌斑生物膜的影響。 方法：SBMP粘接系統(tǒng)作為本實(shí)驗(yàn)的對(duì)照組。NAg按質(zhì)量分?jǐn)?shù)0.1%被添加到對(duì)照粘接劑和底膠中。NACP則按質(zhì)量分?jǐn)?shù)10％，20％，30％和40％與對(duì)照粘接劑混合。使用人唾液培養(yǎng)所得到牙菌斑全菌生物膜模型來(lái)研究生物膜，讓其附著在由復(fù)合樹(shù)脂，粘接劑和底膠構(gòu)成的試件上進(jìn)行生長(zhǎng)。測(cè)定了牙菌斑生物膜的代謝活性，CFU計(jì)數(shù)和產(chǎn)乳酸量。 結(jié)果：人牙本質(zhì)剪切粘接強(qiáng)度介于26至34兆帕間，說(shuō)明添加了NAg和NACP后粘接強(qiáng)度沒(méi)有顯著下降（P0.1）。與對(duì)照組相比，添加了NAg和NACP牙本質(zhì)粘接劑和底膠大大減少了生物膜活力和代謝活性。添加了NAg和NACP的實(shí)驗(yàn)組全菌，總鏈球菌，變形鏈球菌CFU計(jì)數(shù)較對(duì)照組降低了近一個(gè)數(shù)量級(jí)。添加了NAg和NACP的實(shí)驗(yàn)組產(chǎn)乳酸量減少到對(duì)照組的1/4。 SEM觀(guān)察發(fā)現(xiàn)牙本質(zhì)小管內(nèi)充填有大量樹(shù)脂突，并且牙本質(zhì)小管和粘接劑層內(nèi)都滲透了大量的NACP。 意義：本研究第一次證實(shí)了含有NAg和NACP的粘接劑可以顯著降低菌斑生物 膜活力和產(chǎn)乳酸量，并且不損害牙本質(zhì)粘接強(qiáng)度。這種添加NAg和NACP的方法可能在其他牙本質(zhì)粘接系統(tǒng)中同樣具有廣泛的應(yīng)用前景。 第三部分含有新型抗菌季銨鹽單體甲基丙烯酸十二烷基二甲銨（dimethylaminododecyl methacrylate, DMADDM）的牙本質(zhì)粘接系統(tǒng) 目的：樹(shù)脂修復(fù)失敗的主要原因是菌斑生物膜產(chǎn)酸引起的繼發(fā)齲。修復(fù)失敗的再修復(fù)花費(fèi)的時(shí)間占到牙醫(yī)操作時(shí)間的50-70%。本研究的目標(biāo)是把新的季銨鹽單體DMADDM和納米銀顆粒NAg添加到牙本質(zhì)粘接劑和底膠中，探討其對(duì)粘接系統(tǒng)抗菌性能和粘接強(qiáng)度的影響。 方法：SBMP粘接系統(tǒng)作為本實(shí)驗(yàn)的對(duì)照組。合成DMADDM并將其與NAg添加到粘接劑和底膠中。使用人唾液培養(yǎng)所得到牙菌斑全菌生物膜模型來(lái)研究生物膜，檢測(cè)生物膜代謝活力，CFU計(jì)數(shù)，產(chǎn)乳酸量，并測(cè)量人牙本質(zhì)剪切粘接強(qiáng)度。 結(jié)果：DMADDM的最低抑菌濃度（minimal inhibitory concentration, MIC）和最低殺菌濃度（minimal bactericidal concentration, MBC）較原先的QADM降低了多個(gè)數(shù)量級(jí)。未固化的加入DMADDM的底膠，其瓊脂平板抑菌環(huán)的直徑遠(yuǎn)大于加入QADM的底膠所形成的抑菌環(huán)直徑（P0.05）。而固化的加入了DMADDM-NAg的粘接劑和底膠大大降低了菌斑生物膜代謝活性（P 0.05）。同時(shí)加入DMADDM和NAg的實(shí)驗(yàn)組，CFU計(jì)數(shù)的結(jié)果少于單獨(dú)加入DMADDM的實(shí)驗(yàn)組（P0.05）。與對(duì)照組相比，加入了DMADDM-NAg的實(shí)驗(yàn)組，菌斑生物膜產(chǎn)乳酸量減少了20倍。在粘接系統(tǒng)中加入DMADDM和NAg對(duì)牙本質(zhì)粘接強(qiáng)度沒(méi)有不利影響。 意義：本研究合成了一種新的抗菌單體DMADDM，并第一次將其添加到牙本質(zhì)粘接劑和底膠中�？咕辣举|(zhì)粘接劑在抑制殘留細(xì)菌和阻止細(xì)菌入侵方面有很重要的作用。DMADDM和NAg在牙本質(zhì)粘接系統(tǒng)和復(fù)合樹(shù)脂修復(fù)方面，有良好的應(yīng)用前景。 第四部分水老化對(duì)含有新型單體dimethylaminododecyl methacrylate的牙本質(zhì)粘接劑粘接強(qiáng)度和抗生物膜活性的影響 目的：本研究的目的是將新的抗菌單體DMADDM以及納米銀顆粒NAg和無(wú)定形磷酸鈣納米顆粒NACP添加到牙本質(zhì)粘接系統(tǒng)中，開(kāi)發(fā)出新的具有抗菌性能的牙本質(zhì)粘接系統(tǒng)，并第一次通過(guò)6個(gè)月的水老化方法，檢測(cè)其牙本質(zhì)粘接強(qiáng)度和抗菌性能的長(zhǎng)期效果。 方法：檢測(cè)了以下四組粘接系統(tǒng)：SBMP對(duì)照組；SBMP+5％DMADDM；SBMP+5％DMADDM+0.1％NAg和SBMP+5％DMADDM+0.1％NAg，粘接劑另加入20％NACP。試件在37℃下水老化1天和6個(gè)月，然后測(cè)量牙本質(zhì)的剪切粘接強(qiáng)度。使用人唾液培養(yǎng)所得到牙菌斑全菌生物膜模型來(lái)研究生物膜，并測(cè)量生物膜代謝活性，CFU計(jì)數(shù)，和產(chǎn)乳酸量。 結(jié)果：SBMP對(duì)照組經(jīng)過(guò)6個(gè)月的水老化后，牙本質(zhì)粘接強(qiáng)度降低了35％（n=10），相比之下，加入抗菌粘接劑的實(shí)驗(yàn)組沒(méi)有出現(xiàn)粘接強(qiáng)度下降。含有DMADDM-NAg-NACP的實(shí)驗(yàn)組表現(xiàn)出了強(qiáng)的DMADDM抗菌效果，菌斑生物膜活力大大降低，代謝活動(dòng)和產(chǎn)酸均顯著減少。與對(duì)照組相比，CFU計(jì)數(shù)減少超過(guò)兩個(gè)數(shù)量級(jí)。此外，含有DMADDM-NAg-NACP的粘接系統(tǒng)具有長(zhǎng)期的抗菌性能，1天和6個(gè)月的抗菌效果沒(méi)有顯著差異（P0.1）。 結(jié)論：添加DMADDM-NAg-NACP的牙本質(zhì)粘接系統(tǒng)具有強(qiáng)效和持久的抗菌性能，經(jīng)過(guò)6個(gè)月水老化后的粘接強(qiáng)度遠(yuǎn)大于商品化對(duì)照組。這種新型抗菌粘接系統(tǒng)能有效抑制菌斑生物膜的生長(zhǎng)和修復(fù)體邊緣的繼發(fā)齲。本方法在其他牙本質(zhì)粘接系統(tǒng)，正畸粘接劑和復(fù)合樹(shù)脂的改性方面具有廣泛的適用性。
[Abstract]:Composite resin and its bonding system have been widely used in repairing tooth defects and improving tooth appearance because of their excellent aesthetic effects and simple clinical operation. But compared with other dental restorative materials, composite resins are more likely to accumulate the biofilm on the surface of the dental plaque, and the polymerization shrinkage and bonding of the composite resin. It is easy to lead to marginal microleakage, which is the channel of saliva and bacteria entering and out, that is, the invasion pathway of plaque biofilm. The plaque biofilm is the main cause of secondary caries and failure to repair. On the one hand, it will directly cause some oral and soft tissue infectious diseases, such as secondary caries, denture stomatitis, and on the other hand it can cause material aging. Such a vicious cycle will eventually cause failure to repair and even have a bad effect on the whole body. The time taken to repair the failed repair takes up to 50-70% of the dentist's operation time, and the cost of repairment in the United States is more than 20 billion dollars a year. There is no antibacterial effect of resin. It is particularly necessary to give the composite resin itself, and the antibacterial effect of the adhesive system which adhesive to the tooth body. The composite resin and adhesive system with antibacterial properties can reduce the effect on the microecological environment of the mouth, improve the long-term clinical effect of the restorations and maintain the microecological environment of the oral cavity. Health. A great deal of research has been made in the development and development of composite resins and bonding systems with antibacterial effects, in order to inhibit the growth of bacteria, prevent the adhesion of plaque biofilms, prevent the occurrence of secondary caries, prevent the failure of repair and the infection and inflammation caused by the restorations.
This topic is mainly studied from the following four parts:
The first part is the development and detection of antibacterial adhesive system: the effect of quaternary ammonium salt and nano silver particles modified dentin adhesive on bonding strength and plaque biofilm.
The second part is to add amorphous calcium phosphate nanoparticles to give the adhesive remineralization ability: a new dentin adhesive containing nano silver and amorphous calcium phosphate.
The third part is the effect of alkyl chain length: a dentin bonding system containing a new antibacterial quaternary ammonium monomer, methacrylic acid, twelve alkyl, two methylamine.
The fourth part is the long-term effect: the effect of water aging on the mechanical properties and antibacterial properties of the antibacterial adhesive system.
Part one: effect of quaternary ammonium salt and nano silver particles modified dentin adhesive on bonding strength and plaque biofilm.
Objective: antibacterial dentine adhesives play an important role in inhibiting residual bacteria and preventing bacterial invasion. The purpose of this study is to develop an antiseptic dentin that contains a new quaternary ammonium salt monomer (quaternary ammonium dimethacrylate, QADM) and nano silver particles (nanoparticles of silver, NAg). The effects of adhesive and base glue containing QADM-NAg on dentin bonding strength and plaque biofilm were studied.
Methods: the commercial dentin adhesive and the bottom glue Scotchbond Multi-Purpose were used as the control group in this experiment. The adhesive and bottom glue in the experimental group were tested in the control group by adding QADM and NAg. to the 10 groups of human dentin shear adhesion strength (n=10). Xie activity, colony forming unit (CFU) count, lactoacid production, dead / live bacteria staining (n=6).
Results: the dentin adhesive and bottom glue added QADM and NAg, the dentin shear bond strength did not decrease, still between 30 and 35 MPa (P0.1). The scanning electron microscope (SCANNINGELECTRON microscope, SEM) photo showed a large number of resin process formation, which was the same in the control group and the experimental group adding QADM and NAg. Compared with the control group, the metabolic activity of the plaque biofilm with the addition of QADM and NAg was significantly reduced. The addition of QADM and NAg to the adhesive was stronger than the addition of a single antibacterial component (P0.05). Compared with the control group, adding QADM and NAg to the adhesive and the bottom glue had the strongest antibacterial activity, and the maximum decreased. The metabolic activity of plaque biofilms decreased the CFU count and the milk yield of an order of magnitude.
Significance: on the premise of not affecting dentin adhesion strength and resin process, this study first confirmed the dentin adhesives and sealant containing QADM and NAg, and has strong antibacterial effect on dental plaque biofilms. Dentine adhesives and sealant containing QADM and NAg are used to inhibit residual bacteria in pit holes and prevent bacterial invasion. It plays an important role in preventing secondary caries..QADM and NAg can also be widely applied to other dentin bonding systems.
The second part is a new dentin adhesive containing nano silver and amorphous calcium phosphate.
Objective: antiseptic dentine adhesives play an important role in inhibiting residual bacteria in pit holes and preventing bacterial invasion at the edge of the prosthesis. The release of calcium (Ca) and phosphate radical ions (PO4) has been proved to be able to promote remineralization of diseased teeth. The aim of this study is to make nano silver particles NAg and amorphous calcium phosphate nanoparticles (Ca3[PO4]). 2, nanoparticles of amorphous calcium phosphate, NACP) was added to dentin adhesive to study its effect on dentin adhesion strength and dental plaque biofilm.
Methods: the SBMP adhesive system was used as a control group in the control group, and the.NAg was added to the control binder and the bottom glue according to the mass fraction of 0.1%. The.NACP was mixed with the mass fraction of 10%, 20%, 30% and 40% with the control adhesive. The growth of dental plaque and biofilm was tested. The metabolic activity, CFU count and lactone content of dental plaque biofilm were determined.
Results: the bonding strength of human dentin shear bond was between 26 and 34 MPa, indicating that the adhesion strength of NAg and NACP was not significantly decreased (P0.1). Compared with the control group, the addition of NAg and NACP dentin adhesives and bottom adhesives greatly reduced the bioactivity and metabolic activity of the biofilm. The experimental group, total Streptococcus, and deformable chain with NAg and NACP were added. The CFU count was nearly one order of magnitude lower than that of the control group. The amount of lactic acid produced in the experimental group with NAg and NACP decreased to the 1/4. SEM of the control group and found a large number of resin processes filled in the dentinal tubules, and a large amount of NACP. was permeated in the dentinal tubules and the adhesive layer.
Significance: This study confirms for the first time that the adhesives containing NAg and NACP can significantly reduce plaque organisms.
Membrane activity and milky acid content, and do not damage dentin adhesion strength. This method of adding NAg and NACP may also have extensive application prospects in other dentin bonding systems.
The third part contains the dentin bonding system of a new antibacterial quaternary ammonium salt monomer, dimethylaminododecyl methacrylate (DMADDM), twelve methacrylic acid (DMADDM).
Objective: the main reason for the failure of resin repair is secondary caries caused by acid production of plaque biofilm. The cost of repairing failed repair is the 50-70%. of dental operation time. The aim of the study is to add the new quaternary ammonium salt DMADDM and nano silver particle NAg to dentin adhesive and bottom glue, and to discuss the resistance to the adhesive system. The effect of bacterial performance and adhesion strength.
Methods: the SBMP adhesive system was used as the control group in this experiment. DMADDM was synthesized and added with NAg to the adhesive and bottom glue. The whole bacterial biofilm model of dental plaque was used to study the biofilm by human saliva culture. The metabolic activity of biofilm, the count of CFU, the milk yield and the shear bond strength of human dentin were measured.
Results: the minimum inhibitory concentration (minimal inhibitory concentration, MIC) and the lowest bactericidal concentration (minimal bactericidal concentration, MBC) of DMADDM decreased more than one order of magnitude compared with the original QADM. The diameter of the agar plate bacteriostasis ring was far greater than the inhibitory ring formed by the bottom glue adding QADM. Diameter (P0.05). However, the metabolic activity of plaque biofilm (P 0.05) was greatly reduced by the addition of DMADDM-NAg adhesive and bottom glue. At the same time, the result of CFU count was less than that of the experimental group adding DMADDM alone (P0.05) with the addition of DMADDM and NAg. Compared with the control group, the experimental group was added to the DMADDM-NAg experimental group and the production of Lactobacillus in the plaque biofilm decreased. 20 times. The addition of DMADDM and NAg to the adhesive system did not adversely affect the bonding strength of dentin.
Significance: a new antibacterial monomer, DMADDM, was synthesized and added to dentin adhesives and adhesives for the first time. Antibacterial dentine adhesives have an important role in inhibiting residual bacteria and preventing bacterial invasion..DMADDM and NAg have good application prospects in dentin bonding system and restoration of complex resin.
The fourth part is the effect of water aging on bonding strength and anti biofilm activity of dentin adhesive containing new monomer dimethylaminododecyl methacrylate.
Objective: the aim of this study was to add new antibacterial monomer DMADDM, nano silver particles NAg and amorphous calcium phosphate nanoparticles NACP into dentin bonding system and develop new antibacterial dentin bonding system. The dentin bonding strength and antibacterial properties were detected for the first time through 6 months of water aging method. The long-term effect.
Methods: the following four groups of adhesive systems were detected: SBMP control group, SBMP+5%DMADDM, SBMP+5%DMADDM+0.1%NAg and SBMP+5%DMADDM+0.1%NAg, and the adhesive was added to the 20%NACP. specimen for 1 days and 6 months at 37, and then the shear bond strength of dentin was measured. The whole bacterial biofilm of dental plaque was obtained by using human Tuo Yepei. Models were used to study biofilms, and to measure biofilm metabolic activity, CFU counts, and lactol production.
Results: after 6 months of water aging in the SBMP control group, the dentin bonding strength decreased by 35% (n=10). In contrast, the experimental group adding antibacterial adhesive did not decrease the adhesion strength. The experimental group containing DMADDM-NAg-NACP showed a strong DMADDM antibacterial effect, the activity of the plaque biofilm was greatly reduced, the metabolic activity and the acid production were all Significantly less. Compared with the control group, the CFU count decreased by more than two orders of magnitude. In addition, the adhesive system containing DMADDM-NAg-NACP had long-term antibacterial properties, and there was no significant difference between 1 days and 6 months of antibacterial effect (P0.1).
Conclusion: the dentin bonding system with DMADDM-NAg-NACP has strong and lasting antibacterial properties. The adhesion strength after 6 months of water aging is much greater than that of the commercialized control group. This new antibacterial adhesive system can effectively inhibit the growth of plaque biofilm and repair the caries on the edge of the prosthesis. This method is used in other dentin bonding systems, The modification of orthodontic adhesive and composite resin has wide applicability.
【學(xué)位授予單位】：首都醫(yī)科大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2013
【分類(lèi)號(hào)】：R783.1

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