Determination of Pesticides, Mycotoxins and Glyceryl Trioleatein in Coicis Semen by GC/LC-Q-TOF/MS

In this study, the analytical method for determination of 33 pesticides (53 compounds), 8 mycotoxins and a quality marker (glyceryl trioleatein) of Coicis Semen was developed by GC/LC-Q-TOF/MS coupled with solid phase extraction, which provided an accurate and efficient manner of detection in order to guarantee the quality and safety of Coicis Semen . For pesticides and mycotoxins, the samples were extracted with 5% formic acid in water-acetonitrile, shook in an ice bath, and cleaned up by PRiME HLB. Among the 61 contaminants, 37 of those determined by liquid chromatography and 40 of those by gas chromatography, which performed good linearity (R ² ＞0.9832). The limits of quantification (LOQ) of 61 compounds determined by the two methods were lower than 0.05 mg/kg. The recoveries of 37 compounds determined by LC and 40 compounds determined by GC at three spiked levels (LOQ, 2×LOQ, and 10×LOQ) were in the range of 70%-120% with RSDs ＜20%. For glyceryl trioleatein, the samples were extracted with acetonitrile directly. the LOQ was 0.2 ng/mL, and it showed good linearity (R ² =0.9998) within the range of 0.5 to 100 ng/mL. The recovery and RSD were 103.8%, and 4.7% (n = 6), respectively. It indicated that the method could determine the pesticide residues, mycotoxins and quality marker, which integrated instruments and shortened the time of pretreatment, with the determination efficiency improved.