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Fig 1.

Extracellular ATP upregulates the expression of MRP2 in enterocyte-like Caco-2 cells.

Human intestinal adenocarcinoma Caco-2 cells were stimulated with 100 μM ATP for 3 or 6 h, or with control vehicle only (Ctrl). (A) Stimulation with ATP significantly increased ABCC2 gene expression (encodes for MRP2) by 1.5 to 2-fold compared to non-stimulated Ctrl as determined by qRT-PCR analysis. Results are presented as the mean ± SEM of five individual experiments performed in duplicate. Statistical significance was determined by one-way ANOVA with Dunnett's multiple comparison post-test. * p < 0.05, ** p < 0.01 as compared with Ctrl. (B) Typical Western blot result is showing enhanced MRP2 expression in ATP-stimulated cells. (C) Densitometric analysis revealed that 100 μM ATP induced MRP2 protein expression by more than 1.5-fold after 6 and 18 h of stimulation compared with control (Ctrl). Results are presented as the mean ± SEM of five separate experiments. Statistical significance was determined by one-way ANOVA with Dunnett's multiple comparison post-test. * p < 0.05 as compared with Ctrl.

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Fig 2.

ATP-dependent stimulation of MRP2 protein expression is strongly reduced in the presence of the P2 receptor antagonist Suramin.

Caco-2 cells were treated with 100 μM PPADS or Suramin 30 min prior to the addition of 100 μM ATP for 6 h. MRP2 expression was analyzed by Western blotting. ATP stimulated the expression of MRP2 as compared to non-stimulated (N-S) cells, whereas the addition of Suramin prior to the ATP stimulation strongly decreased MRP2 expression compared to ATP-stimulated cells in the presence of vehicle (DMSO (-)) only. The presented blot is typical of three separate sets of experiments.

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Fig 3.

MRP2 expression is regulated by MEK/ERK signaling cascade.

Caco-2 cells were pretreated with NFκB (2 μM, Bay, BAY11-7082), MEK1/2 (10 μM, U0, U0126), PI3K (20 μM, LY, LY294003) and p38 (20 μM, SB, SB203580) inhibitors for 30 minutes and stimulated with 100 μM ATP for 6 h. (A) A typical Western blot against MRP2 is displayed from which (B) densitometry analysis showed a significant reduction in MRP2 expression in the presence of U0126, a selective MEK 1/2 inhibitor. Cells pretreated with U0126 led to a 75% reduction in the expression of MRP2 compared to ATP-stimulated cells only (-). Results are presented as the mean ± SEM of three separate experiments performed in duplicate. Statistical significance was determined by an unpaired t-test, where * p < 0.05 vs. non-stimulated (N-S) or ATP-stimulated cells as indicated on figure.

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Fig 4.

Stimulation of Caco-2 cells with ATP increases resistance to the anti-cancer drug etoposide.

Caco-2 cells were incubated with increasing concentrations of etoposide for 84 h in the presence or absence of 100 μM ATP added every 24 h. MTT cell viability assay was used to determine sensitivity to the drug. (A) A dose-response curve was fitted to the data to determine the toxicity (IC50 value) of the drug. Results are presented as a non-linear survival curve of a typical response. (B) IC50 and RR values are presented on the histogram and results represent the means ± SEM of three to four independent experiments performed in triplicate. Statistical significance was determined by unpaired t-test, where * p < 0.05 as compared with Ctrl.

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Fig 5.

The down-regulation of MRP2 expression by shRNA renders Caco-2 cells more sensitive to etoposide.

(A) Western blot analysis was used to assess the down-regulation of MRP2 protein expression in the presence of two shRNAs directed against the protein. Down-regulation was achieved by lentiviral infection of Caco-2 cells as previously described [31]. shRNA directed against MRP2 (sh305 and sh307) abolished protein expression by 90–100% comparatively to cells expressing a non-targeting shRNA (shNT). (B) Caco-2 cells stably expressing shNT or shMRP2 (#305) were incubated with the cytotoxic drug etoposide for 84 h. Sensitivity to the anti-cancer drug was determined by the MTT cell viability assay. A dose-response curve was fitted to the data to determine the toxicity (IC50 value) of the drugs. The non-linear survival curves are presented as the mean ± SEM of four experiments performed in triplicate. Statistical significance was calculated using multiple t-test comparisons, where * p < 0.05 as compared with shNT. Inhibition of human shMRP2 expression reduced the resistance of Caco-2 cells to etoposide compared to control cells. IC50 and RR values are presented in Table 1.

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Table 1.

IC50 and relative resistance (RR) values measured in response to etoposide, cisplatin and doxorubicin treatment of Caco-2 cells stably expressing non-target shRNA (shNT) or shMRP2.

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