Furthermore, the sustained oxidative stress progressed to trigger apoptosis through mitochondrial dysfunction in tier 3. Therefore, mitochondrial superoxide production and mitochondrial membrane depolarization of PS NPs-treated BEAS-2B cells were detected by MitoSox Red and JC-1 staining assay. Figure
3G and Fig. S8 illustrate that red fluorescence intensity of MitoSox was progressively increased with higher PS NPs concentrations, indicating that PS NPs resulted in the accumulation of mitochondrial superoxide in BEAS-2B cells. Meanwhile, the depolarization of mitochondrial membrane potential (Δψ
m) serves as a hallmark event in early apoptotic activity. In healthy cells, the higher Δψ
m causes JC-1 to appear in cells in the form of aggregates and emits red fluorescence. When Δψ
m decreases, JC-1 shifts to its monomeric form and shows green fluorescence. Therefore, a drop in Δψ
m could be measured by the ratio of green/red fluorescence of JC-1 [
42]. As shown in Fig.
3H and Fig. S9, untreated BEAS-2B cells mainly exhibited predominant red fluorescence from JC-1 aggregates, indicative of a high Δψ
m. On the contrary, green fluorescence from JC-1 monomer appeared in PS NPs-treated BEAS-2B cells and the intensity of green fluorescence was increased when the concentration of PS NPs was raised from 60 to 1,000 μg/ml, indicating that PS NPs reduced Δψ
m in a dose-dependent manner. In fact, Δψ
m is crucial to maintain the physiological function of the respiratory chain. Thus, the real-time oxygen consumption rate (OCR), an indicator of mitochondrial respiration, was monitored by XFe seahorse systems. Figure
3I reveals a dose-dependent inhibition effect of PS NPs in the mitochondrial stress profiles in BEAS-2B cells. Basal respiration was reduced by 41.0 ± 10.44% when the concentration of PS NPs reached 1,000 μg/ml, accompanied by remarkable reductions in proton leak (12.8 ± 2.07%) and maximal respiratory capacity (46.7 ± 10.92%) (Fig. S10). In contrast, OCR linked to adenosine triphosphate (ATP) production showed a transient increase at lower concentrations attributed to mild uncoupling, followed by a graded decline as the electron transport chain became impaired (Fig.
3J). These observations illustrated a dynamic transition from a compensatory state to decompensated state in the process of ATP production. Taken together, PS NPs induced mitochondrial dysfunction in BEAS-2B cells. Finally, apoptosis represents the terminal outcome of oxidative stress injury, which was analyzed by Annexin V–fluorescein isothiocyanate (FITC)/propidium iodide (PI) double staining. Figure
3K displayed that PS NPs induced apoptosis in a dose-dependent manner, confirming the activation of cell death pathways. Bcl-2, a pivotal anti-apoptotic protein that preserves the integrity of the mitochondrial outer membrane [
43,
44], was further examined to substantiate the mechanistic connection between mitochondrial damage and cell apoptosis. As shown in Fig. S11, Bcl-2 protein expression decreased progressively with increasing PS NP concentrations, corroborating the activation of the mitochondrial-dependent apoptotic pathway. All considered, these findings indicate that PS NPs induced hierarchical oxidative stress responses in BEAS-2B cells, evolving from adaptive antioxidant activation to oxidative damage, mitochondrial collapse, and apoptotic cell death. This stepwise progression provides a compelling mechanistic explanation for the observed cytotoxicity, underscoring hierarchical oxidative stress as the central pathway mediating PS NPs-induced pulmonary toxicity. These results are consistent with previous studies reporting that oxidative stress-mediated mitochondrial dysfunction constitutes a major mechanism of nanoplastic cytotoxicity [
45]. The observed Bcl-2 down-regulation parallels the collapse of mitochondrial membrane potential and subsequent cytochrome c release reported in other polymeric nanoparticle systems [
46–
48].