Polyvinyl alcohol/polyacrylic acid (PVA/PAA) bilayer hydrogel nanofibres were successfully fabricated by electrospinning and physically crosslinked via heat treatment. The effects of the thermal annealing process on the structure, morphology, swelling, thermal properties and hydrophilicity of electrospun nanofibres were investigated. In addition, these membranes were also used to incorporate doxorubicin and clarithromycin for osteosarcoma treatment, one in each layer. These drugs were used because it is hypothesized in this work that a synergism occurs between both drugs. So, these membranes were analyzed towards their dual-drug release and potential cytotoxicity towards the U2OS human osteosarcoma cell line. Moreover, the water contact angle, disintegration, swelling and weight loss studies confirmed the rapid swelling and improved water stability of the annealed PVA/PAA bilayer nanofibres. The annealed bilayer nanofibres exhibited an increase in the average diameter and degree of crystallinity. In addition, the results revealed that a variation occurred in the degree of hydrophilicity of annealed PVA/PAA bilayer nanofibres. The PAA nanofibres surface exhibited higher hydrophilicity than the PVA nanofibres surface. Drug delivery presented to be as fast rate release for clarithromycin and slow-rate release for doxorubicin, which may be advantageous because both drugs exhibited to be synergetic for certain dosages presenting the combination of the drugs higher than 50% of cell inhibition, while these membranes had higher inhibition values (up to 90%), which was attributed to the PAA but also the drugs. These unique properties are of potential interest in drug delivery applications for dual drug delivery where the tunability of surfaces is desirable.

聚乙烯醇/聚丙烯酸（PVA/PAA）双层水凝胶纳米纤维通过静电纺丝和热处理物理交联成功制备。研究了热退火过程对电纺纳米纤维的结构、形貌、溶胀、热性能和亲水性的影响。此外，这些膜还用于掺入多柔比星和克拉霉素用于治疗骨肉瘤，每层一个。使用这些药物是因为在这项工作中假设两种药物之间会发生协同作用。因此，对这些膜的双重药物释放和对 U2OS 人骨肉瘤细胞系的潜在细胞毒性进行了分析。此外，水接触角、崩解、溶胀和失重研究证实了退火的 PVA/PAA 双层纳米纤维的快速溶胀和改善的水稳定性。退火的双层纳米纤维表现出平均直径和结晶度的增加。此外，结果表明，退火后的 PVA/PAA 双层纳米纤维的亲水性程度发生了变化。PAA 纳米纤维表面比 PVA 纳米纤维表面表现出更高的亲水性。药物递送表现为克拉霉素的快速释放和多柔比星的缓慢释放，这可能是有利的，因为这两种药物在某些剂量下表现出协同作用，呈现出高于 50% 的细胞抑制的药物组合，而这些膜具有更高的抑制值（高达 90%），这归因于 PAA，也归因于药物。