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Western Blot Analysis of Protein Phosphorylation

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Example 4

Cells were treated with experimental compound for 12 hrs then lysed in either NP-40 lysis buffer (50 mM Tris-HCl pH 8.0, 150 mM NaCl, 1% NP-40) or RIPA lysis buffer (50 mM Tris-HCl pH 8.0, 150 mM NaCl, 1% NP-40, 0.25% sodium deoxycholate, 1 mM EDTA) containing protease and phosphatase inhibitors (Roche). Lysates were centrifuged at 17000×g for 12 minutes and the supernatant was collected for immunoblot analysis. Equal amounts of protein were separated by SDS-PAGE on pre-cast 2-20% polyacrylamide gradient gels (Biorad) and electroblotted onto Immobilin poly-vinyl difluoride (PVDF) membrane (EMD Millipore). Membranes were blocked in TBS-T (50 mM Tris-HCl, pH 7.5, 150 mM NaCl, 0.1% Tween-20) containing 5% non-fat dry milk for 1.5 hours at room temperature, followed by overnight incubation with primary antibodies diluted in blocking buffer at 4° C. (anti-N17-S13pS16p 1:2500; anti-p53-S392p 1:1500; anti-GAPDH 1:7500). After three 15-minute TBS-T washes, membranes were incubated with HRP-conjugated secondary antibodies diluted in blocking buffer (1:50000) for 45 minutes at room temperature, and visualized using Immobilin enhanced chemiluminescence HRP substrate (EMD Millipore) on a MicroChemi system (DNR Bio-imaging Systems). Bands were quantified using NIH Image J software and normalized to GAPDH controls (FIG. 4).

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2

Western Blot Analysis of MMP9 Expression

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Samples were lysed using radioimmunoprecipitation assay (RIPA) lysis buffer (Thermo Scientific, Waltham, MA, USA) with protease and phosphatase inhibitor cocktail (Roche Holding AG, Basel, Switzerland) and centrifuged at 4°C and 14,000 g for 20 min. The supernatant was collected, and protein concentration was determined using a BCA kit (Thermo Scientific). The same amount of protein for each sample (20 μg) was loaded on a polyacrylamide gel (10%). Proteins were separated by SDS-PAGE and electro-transferred to PVDF membranes (Bio-Rad). Membranes were blocked using 5% skim milk in PBS with 0.25% Tween-20 (PBST), and subsequently incubated at 4°C overnight with anti-MMP9 (1:1,000; Abcam, ab38898) or β-actin (1:5,000; Thermo Scientific, MA5–15739) antibodies. After washing, membranes were bound to HRP-conjugated secondary antibodies [Donkey IgG anti-rabbit (1:2,000; Cell Signaling Technology, Beverly, MA, USA, 7074s) or anti-mouse (1:2,000; Cell Signaling Technology, 7076s)] and incubated at room temperature for 1 h. Blots were developed using enhanced chemiluminescence (ECL) Western blotting detection reagent (Thermo Fisher Scientific) and analyzed using a MicroChemi system (DNR Bio-imaging Systems, Neve Yamin, Israel).
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Western Blot Analysis of Primary Chondrocytes

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The proteins from the primary chondrocyte cultures (n = 3 independent isolations) were harvested using 300 µL RIPA buffer supplemented with protease and phosphatase inhibitors (Roche Diagnostics, Indianapolis, IN). The total cell lysates (containing 20–30 µg protein) were separated by 10% SDS-polyacrylamide gel electrophoresis and transferred to polyvinylidene difluoride membranes (Immobilon-P; Millipore Corporation, Billerica, MA, USA). The membranes were then blocked using 5% skimmed milk in PBS with 0.25% Tween-20 (PBST) and incubated at 4 °C overnight with the primary antibodies listed in Supplementary Materials Table S2. After washing with PBST, the membranes were bound to horseradish peroxidase-conjugated secondary antibodies and incubated at RT for 2 h. After washing with PBST, the blots were developed using enhanced chemiluminescence Western blotting detection reagent (Thermo Fisher Scientific, Waltham, MA, USA) and analyzed with the MicroChemi system (DNR Bio-imaging Systems, Neve Yamin, Israel). The Western blot band intensities were quantified with ImageJ software. A list of the primary antibodies used for the Western blot analysis are shown in Supplementary Materials Table S2.
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4

Chicken Immunoglobulin Detection Protocol

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Immunoglobulins were detected using: goat‐anti‐chicken‐IgM‐HRP (Bethyl), goat‐anti‐chicken‐IgY‐HRP (Jackson ImmunoResearch Laboratories), and goat‐anti‐chicken IgA (Bethyl). Blots were developed with ECL substrate (GE Healthcare) and signal detected using the MicroChemi System (DNR Bio‐Imaging Systems).
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