1. Background
2. Objectives
3. Methods
3.1. Reagents
3.2. Cytotoxicity Experiments
3.3. Immunofluorescence
3.4. Bioinformatics Analyses
3.5. ELISA Assays
3.6. In-cell Western
3.7. Statistical Analysis
4. Results
4.1. Bidirectional Modulation of Sorafenib-Induced HepG2 Cell Inhibition by Celastrol at Varied Concentrations
Bidirectional modulation of sorafenib-induced HepG2 cell inhibition by celastrol at varied concentrations. A, tumor cells were exposed to sorafenib alone or in combination with various high concentrations of celastrol (1, 2, 4, or 8 μmol/L) for 72 h before being subjected to MTT assay. At concentrations greater than 2 μmol/L, celastrol enhanced the sorafenib-induced cytotoxicity to hepatocellular carcinoma (HCC) cells; B, tumor cells were exposed to sorafenib alone or in combination with low concentrations of celastrol (0.05, 0.1, 0.2, or 0.5 μmol/L) for 72 h before being subjected to MTT assay. Celastrol dose-dependently inhibited the sorafenib-induced cytotoxicity to HCC cells; C, LO2 cells were exposed to sorafenib alone or in combination with high concentrations of celastrol (1, 2, 4, or 8 μmol/L) for 72 h before being subjected to MTT assay. At concentrations greater than 4 μmol/L, celastrol enhanced the cytotoxicity induced by sorafenib toward LO2 cells; D, LO2 cells were exposed to sorafenib alone or in combination with low concentrations of celastrol (0.05, 0.1, or 0.2 μmol/L) for 72 h before being subjected to MTT assay. Sorafenib was not cytotoxic when administered alone as in combination with celastrol; E, tumor cells were pretreated with 0.4 μm sorafenib for 48 h, washed twice, and retreated with 0.4 μm sorafenib for another 48 h; F, tumor cells were pretreated with 0.4 μm sorafenib and celastrol (0.2 or 8 μm) for 48 h, washed twice, and retreated with 0.4 μm sorafenib for another 48 h. MTT assays were tested to evaluate the cytotoxic effects in HepG2 cells (Abbreviations: Sor, sorafenib; cel, celastrol; NS, not significant. *P < 0.05, **P < 0.01).
4.2. Low-Concentration Celastrol Reversed Sorafenib Resistance by Altering the Secretory Profile of HepG2 Cells
Low-concentration celastrol reversed sorafenib resistance by altering the secretory profile of HepG2 cells. A, effects of various conditioned media (CM) on tumor cell viability after exposure to 0.4 μm sorafenib for 48 h; B, pH of different CM was measured using a pH meter; C, effects of various CM subjected to repeated freeze-thawing on tumor cell viability after exposure to 0.4 μm sorafenib for 48 h. Gene set enrichment analysis (GSEA) results demonstrated that the pathways enriched included the cytokine-biosynthetic process; and E, IL6 signaling pathway; F, the volcano plot, based on Gene Expression Omnibus (GEO) data, showed the up-regulated expression level of IL6 in the sorafenib-treated HepG2 cells (abbreviations: Sor, sorafenib; cel, celastrol; NS, not significant. *P < 0.05, **P < 0.01).
4.3. IL-6-Modulated Resistance of Hepatocellular Carcinoma Cells to Sorafenib
IL6 modulated the resistance of hepatocellular carcinoma (HCC) cells to sorafenib. A, tumor cells were treated with 0.4 μm sorafenib and celastrol (0.2 or 8 μm) for 24 h. The IL6 levels in the tumor cells were then determined via immunofluorescence (IF) assays (red: IL6, blue: DAPI, bar = 20 μM); B, tumor cells were treated with 0.4 μm sorafenib and celastrol (0.2 or 8 μm) for 48 h. The IL6 levels in the supernatants were then determined via ELISA assays; C, the IL6 levels in HepG2 and Hep3B cell supernatants were determined via ELISA assay; D, effects of various conditioned media (CM) containing an IL6-neutralizing antibody (1 μg/mL) or exogenous human IL6 (10 ng/mL) on HepG2 cell viability after exposure to 0.4 μm sorafenib for 72 h; E, HepG2 cells were cotreated with 0.4 μm sorafenib and exogenous human IL6 (10 ng/mL) for 72 h, and the cell viability was tested via MTT assay; F, Hep3B cells were cotreated with 0.4 μm sorafenib and an IL6 neutralizing antibody (1 μg/mL) for 72 h, and the cell viability was tested via MTT assay; G, the levels of phosphorylated and total AKT in HepG2 cells after exposure to 0.4 μm sorafenib and 0.2 μm celastrol for 12 h were determined via In-Cell-Western assay; H, effects of LY294002 (1 μg/mL) or SC79 (2 μM) on IL-6 secretion in HepG2 cells after exposure to 0.4 μm sorafenib and 0.2 μm celastrol for 24 h (abbreviations: Sor, sorafenib; cel, celastrol; NS, not significant. *P < 0.05, **P < 0.01).


