基于抗溶胀水凝胶的生物粘合界面和植入器件的研究

水凝胶因其独特的类组织生物、化学和力学特性，广泛应用于药物递送、组织工程、医用粘合剂和植入器件等领域。基于水凝胶的生物粘合剂通过物理或化学作用紧密粘附在组织表面以代替缝合线，可以避免组织损伤、减少手术时间和促进伤口愈合，在外科手术止血、伤口密封和体内植入器件等领域具有重要应用价值。此外，随着基于光递送的光动力治疗、光学传感和光遗传学等领域的发展，柔性可植入水凝胶光纤由于其低光损耗、可拉伸和优异的组织力学适配性等特点，在相关领域得到了广泛研究。

复杂的体内特殊应用场景对水凝胶粘合剂性能具有特定的要求，已有研究缺乏对相关需求的关注，忽视了水凝胶粘合剂在体内复杂的体液环境（如血液、消化液、泪液等）和动态机械载荷下面临的溶胀失效、力学性能下降等问题。针对这些问题，本论文研究从抗溶胀水凝胶设计制备策略出发，通过调控凝胶网络结构来解决水凝胶粘合剂在不同应用环境中的长期稳定性问题。设计并开发了针对跟腱、胃和角膜的特异性水凝胶粘合剂。水凝胶植入器件方面，已有研究开发了光电集成化的水凝胶光纤用于中枢神经光遗传调控，但这类集成器件面临导电物质因吸光特性严重破坏水凝胶光导通路的问题。为了解决这一问题，基于前期的界面粘合调控研究基础，提出了多功能层集成制备策略，成功开发了高性能导光、导电集成化水凝胶光纤，并用于中枢光遗传学调控研究。

主要的研究内容与结论如下：

（1）提出了通过静电作用促进凝胶网络分相和单面功能化策略，用于解决水凝胶粘合剂在跟腱断裂缝合术后修复中面临的体液稳定性差和组织粘连问题。开发了具有体液环境下长期稳定（>168 h）和不对称组织粘合特性（粘合强度相差10倍）的水凝胶粘合剂（Janus Gels, JanuGels）。JanuGels通过干交联机制实现对跟腱组织的高强度粘合（界面韧性> 200 J/m²，粘合强度> 40 kPa），并通过为跟腱提供长期牢固的粘合界面和避免缝合点周围应力集中问题，成功实现跟腱的无组织粘连和显著改善生物力学性能恢复。

（2）针对胃部的低pH胃液环境，提出了通过疏水作用促进凝胶网络相分离，作为稳定的物理交联的耐酸环境溶胀策略，并引入聚合物粘合刷（PAA-NHS），开发了耐酸的水凝胶粘合剂（Acid-tolerant hydrogel bioadhesives, ATGels）。ATGels在极端胃酸条件（pH = 2.0）下能够快速密封胃穿孔（< 2 min）并形成牢固的组织粘合界面（界面韧性> 300 J/m²，粘合强度> 60 kPa），并且表现出了长期的组织粘合酸稳定性（10天粘合强度保留> 70%），成功实现了体内对胃穿孔的无泄漏密封和有效促进组织修复。

（3）针对眼科应用对粘合剂高透明度的要求，在相分离策略的基础上进一步提出了相分离束缚策略以控制相分离尺寸保证水凝胶兼具抗溶胀和高透明度，开发制备了适用于眼科角膜移植中无线缝合的生物胶水（Arrested phase separation bioglue, AGlue）。AGlue具备快速光引发固化（1 min， 405 nm）的特点，同时具有优异的抗溶胀性能（溶胀率< 50%）、高透明度（> 90%，400-800 nm，厚度：100 μm）和强组织粘合作用（粘合强度> 30 kPa，爆破压> 20 kPa）。此外，AGlue还具有与角膜修复适配的体内降解周期（> 30天）和良好的免疫排异相容性，在眼科角膜移植的无线缝合与修复应用中具有广阔的应用前景。

（4）在实现高透明生物胶水开发的基础上，进一步开发了具有导光、导电性能集成化的水凝胶光纤（Integrated hydrogel optical fiber-based electronics, iHOFE）用于中枢光遗传学研究。基于前面的界面粘合调控研究，通过多功能分层（导光层、导电层和绝缘层）集成制备原则，避免了导电聚合物对水凝胶光纤导光通路的影响。iHOFE具有低光损耗（0.45 dB/cm，473 nm）、合适的电生理记录阻抗（80-100 kΩ，1 kHz）和优异的组织力学适配性（杨氏模量：860 kPa）的性能。iHOFE各个功能层间牢固的界面连接（界面韧性> 50 J/m²）保证了其在脑组织微扰动（100 μm）环境下的长期稳定性。在应用方面，将iHOFE成功应用于中枢神经疾病（癫痫）的电生理信号记录和光遗传干预，以及长期植入（2个月）对小鼠焦虑行为学的光遗传学调控研究中。

Hydrogels are similar to biological tissues in biological, chemical, and mechanical properties, and have been widely used in drug delivery, tissue engineering, bioadhesives, and implantable devices. Hydrogel adhesive is a representative example for replacing suture in hemostasis, sealing wound, and rigid device anchorage via physical or chemical bonding. They could effectively mitigate the tissue damage, reduce surgical time, and promote the wound healing. Additionally, with the development of photodynamic therapy, optical sensing, and optogenetics, hydrogel optical fibers exhibit great promise in these fields in light of their distinct transparency, stretchability, and mechanical compliance.

Previous studies mainly focus on the general performance requirements of hydrogels, neglecting the swelling and mechanical deterioration during the direct contact with complex bodily fluids (such as blood, digestive fluids, tears, etc.) as well as the dynamic movement. This thesis develops various anti-swelling hydrogel design and fabrication strategies to improve the long-term stability in specific in vivo conditions. We developed various hydrogels bioadhesives with anti-swelling for Achilles tendon rupture repair, sutureless sealing of gastric perforations and keratoplasty. For the hydrogel-based optic-electronic integrated device, the light-absorbing properties of conductive polymers substantially mitigate the efficiency of light delivery. To solve this challenge, we proposed the multi-functional layer integrate strategy to integrate the light delivery and electrically conducting modules within a single hydrogel device.

The main research contents and result are as follows:

(1) To address the swelling of hydrophilic hydrogel adhesives and tissue adhesion encountered in Achilles tendon repairing, a new strategy was proposed involving electrostatic interactions to promote phase separation and Janus functionalization of hydrogels. This led to the development of asymmetric hydrogel adhesives (JanuGels) with body fluid tolerance (>168 h) and Janus bioadhesion properties (10×). JanuGels achieved tough hydrogel adhesion through the dry-crosslinking mechanism (interface toughness: > 200 J/m², adhesive strength: > 40 kPa). Moreover, JanuGels provided a long-term robust interface with tendon. This hydrogel bioadhesive successfully inhibits undesirable post-surgical adhesion and significantly improves the biomechanical performance of the injured Achilles tendon.

(2) The electrostatic interactions would be disrupted in acid environment, rendering phase separation strategy is unsuitable for gastric repair. This section proposed a hydrophobic interaction induced phase separation of hydrogel (ATGels), exhibiting stable physical crosslinking in extremely acidic fluids.  ATGels exhibit high gastric perforation sealing efficiency (< 2 min), accompanying with tough tissue adhesion properties (interface toughness > 300 J/m², adhesive strength > 60 kPa), and long-term tissue adhesion stability (> 70% after 10 days). The long-term robustness in mechanical and tissue bonding of ATGels enables its successful application for fluid-tight, sutureless sealing of gastric perforations, and promotes repair in a rat model.

(3) To address the demand for high transparency in ophthalmic applications, the formation of large-sized phases (> 40 nm, within the visible light range) would destruct the transparency of hydrogels. This section proposes an arrested phase separation strategy and develops a high transparency and anti-swelling bioglue (AGlue). AGlue features rapid photocrosslinking (1 min, 405 nm) along with excellent anti-swelling (swelling ratio < 50%), high transparency (> 90% at 400-800 nm, thickness: 100 μm), and desirable adhesive strength (adhesive strength > 30 kPa, burst pressure > 20 kPa). Additionally, AGlue possesses an in vivo degradation period adapted for corneal repair (> 30 days) and excellent immunocompatibility, showing potential for sutureless corneal transplantation.

(4) Based on the highly transparent hydrogel bioglue above, this section applies it to the implantable optical devices. A hydrogel-based integrated photoelectronic device (iHOFE) with light waveguides and electroconductivity, is developed through multifunctional layers fabrication. iHOFE effectively avoids the absorption of conductive polymers on the light propagation pathways of hydrogel optical fibers. The device exhibits excellent light delivery efficiency (0.45 dB/cm, 473 nm), appropriate electrophysiological recording impedance (80-100 kΩ, 1 kHz), and tissue mechanics compatibility (Young's modulus: 860 kPa). Robust interfacial connections between different functional layers of iHOFE (interface toughness > 50 J/m²) ensures its enduring stability amid brain micromotions (100 μm). Moreover, iHOFE capable of recording epileptiform activity and optogenetic modulation, as well as for long-term implantation (2 months) in chronic behavioral tests and in vivo neurological modulation.

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