Solvent-saturated solid matrix technique for increasing the efficiency of headspace extraction of volatiles

Due to the slow mass transfer rate of substance in solid media, very limited amount of volatiles can be released from the solid matrix to the headspace in the static headspace analysis. Thus, low sensitivity is often the main problem of static headspace analysis of the volatiles contained in a solid sample. Here, we reported on a solvent-saturated solid matrix (SSSM) technique which successfully enhanced the headspace extraction efficiency, and improved the sensitivity of the headspace analysis of the volatiles in solid sample. By adding a small amount of high-boiling-point solvent (e.g. glycerin) onto the solid sample to form a surface-covered solvent layer, the headspace extraction efficiency can be significantly increased by up to 2.5 times higher than that of the conventional one. Based on the experimental investigation of the performance of different amounts of solvent used for the headspace extraction of volatiles in air-dried lotus flower samples, the possible mechanism for the SSSM assisted headspace extraction has been proposed and validated, which showed that a saturation point of solvent existed for a given amount of solid sample, and the maximum extraction efficiency could be obtained at this saturation point. Moreover, positive results were also achieved when applying this new technique in the headspace extraction of the volatiles to the other two solid samples, which means this newly developed technique may open up a new avenue, and also serve as a general strategy for improving the sensitivity of headspace analysis of the volatiles entrapped in solid matrices.