Rapid and sensitive determination of neomycin and kanamycin in measles, mumps, and rubella vaccine via high-performance liquid chromatography-tandem mass spectrometry using modified super-paramagnetic Fe(3)O(4) nanospheres.

A simple magnetic dispersive solid-phase extraction (MDSPE) methodology based on mesoporous Fe(3)O(4)@ succinic acid nanospheres and high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been developed to determine kanamycin (KNM) and neomycin (NEO) contents in Measles, Mumps, and Rubella (MMR) vaccine products. The monodispersed mesoporous Fe(3)O(4) nanospheres with self-assembled carboxyl terminated shell have been prepared via a simple solvothermal method. These as-synthesized mesoporous Fe(3)O(4) nanospheres showed a high magnetic saturation value (M(s) = 46 emu g(-1)) and large specific surface area (111.12 m(2) g(-1)) which made them potential candidates as sorbents in magnetic solid-phase extraction. The adsorption experimental data fitted well with the Freundlich-Langmuir isotherm and followed a pseudo-second-order kinetic model. Moreover influential parameters on extraction efficiency were investigated and optimized. Under optimal conditions, the limits of detection for KNM and NEO were 1.0 and 0.1 ng mL(-1), respectively. Recovery assessments using real samples exhibited recoveries in the range of 96.0 +/- 4.3 to 101.5 +/- 7.1 %, with relative standard deviations of <10.7% (for intra- day) and <14.6% (for inter- day). The proposed method was successfully applied for different spiked and un-spiked MMR vaccine samples. The presented extraction method provides a fast, selective, robust and practical platform for the detection of KNM and NEO in MMR vaccine samples.