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The samples were then sonicated in ice-cold water using Biorupter UCD-200 sonicator for 5 min (30 s sonication and 30 s rest cycle

doi: 10.7150/thno.49426

At each time point, a 50 l supernatant was collected and the Ex4 concentration was determined by Ex4 EIA Kit (Phoenix Biotech, USA, catalog number: EK-07094) according to the standard protocol