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The separate co‐encapsulation and selective controlled release of multiple encapsulants in a predetermined sequence has potentially important applications for drug delivery and tissue engineering. However, the selective controlled release of distinct contents upon one triggering event for most existing microcarriers still remains challenging. Here, novel microfluidic fabrication of compound‐droplet‐pairs‐filled hydrogel microfibers (C‐Fibers) is presented for two‐step selective controlled release under AC electric field. The parallel arranged compound droplets enable the separate co‐encapsulation of distinct contents in a single microfiber, and the release sequence is guaranteed by the discrepancy of the shell thickness or core conductivity of the encapsulated droplets. This is demonstrated by using a high‐frequency electric field to trigger the first burst release of droplets with higher conductivity or thinner shell …