Vitamin C (VC) is a hydrophilic antioxidant that plays a vital role in the protection of health and is also an integral ingredient in beauty formulations due to its numerous distinct and necessary properties. However, its application in the area of cosmeceuticals still confronts huge challenges relating to its instability and low bioactivity. Therefore, it is necessary to prevent its degradation by utilizing microencapsulation techniques, many and various of which, entailing the use of liposomes, nanoemulsions, lipid particles, and layered double hydroxide, have already been introduced. Nevertheless, such techniques still have several disadvantages in terms of either their difficult preparation or toxicity to skin. Recently, aminoclay (AC), a synthetic organic-nanoclay comprising 3-aminopropyl-functionalized magnesium phyllosilicate, has been proposed as a promising candidate for encapsulation and delivery of active agents in cosmeceuticals. In the present work, a novel magnesium aminoclay/vitamin C (MgAC-VC) hybrid was successfully fabricated by a simple onepot synthesis method via the in situ loading of VC into MgAC. The resultant hybrid was found to highly improve the stability and controllable release of VC. Compared with free VC, the MgAC-VC hybrid exhibited significantly enhanced stability of VC under high temperature (60 °C) as well as slow and controllable release of VC from MgAC-VC hybrids over 24 h. Our results suggest that such MgAC-VC hybrids can potentially be utilized in cosmeceutical applications for delivery of VC and other antioxidants.