Herein, we introduce an original strategy toward one-step encapsulation, storage and controlled release of low molecular weight organic compounds via electroplated nanoparticles. This concept is demonstrated on the basis of the encapsulation of several organic matrices typically used for matrix-assisted laser desorption ionization mass spectrometry (MALDI-MS) as a case study via co-deposition with palladium nanoparticles (Pd-NPs). Remarkably, Pd-NPs act as a capsule for MALDI matrices and thus provide their controlled release depending on the external factors, viz. applied laser fluence or pH of the surrounding media. The proposed approach is considered as a simple, fast and inexpensive preparation method towards the formation of ultimate self-assembled hybrid MALDI matrices with a less pronounced "sweet spot" phenomenon and improved long-term stability.