A procedure based on the QuEChERS methodology and Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) is described, for the determination of Nicotine in mushrooms. QuEChERS methodology was used to determine Ni...A procedure based on the QuEChERS methodology and Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) is described, for the determination of Nicotine in mushrooms. QuEChERS methodology was used to determine Nicotine in dried and fresh mushrooms under basic conditions with primary secondary amino sorbent (PSA) clean up. The chromatography was performed on C 18 reversed phase column using a gradient of acetonitrile and ammonium formiate lmM pH = 3.4 as mobile phase at a flow rate of 0.3 mL min^-1. Nicotine was determined by using Nicotine-d3 as internal standard. Limit of quantification (LOQ) was 0.01 mg kg^-1 for both fresh and dried mushrooms. Calibration curve was linear over the concentration range of 0.01-2.3 mg mL^-1, with r2 〉 0.99. As for recoveries in dried mushrooms, spiking levels of 0.32 mg kg^-1 and 2 mg kg^-1 were considered whereas for the fresh mushrooms the recoveries were determined at 0.036 mg kg^-1 and 0.36 mg kg^-1. Satisfactory results were obtained for both matrices and the recoveries proved to range from 105% to 135%, with a standard deviation in the range 17-20. The method was applied to the analysis of Nicotine to assess the levels of nicotine in fresh and dried mushrooms.展开更多
文摘A procedure based on the QuEChERS methodology and Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) is described, for the determination of Nicotine in mushrooms. QuEChERS methodology was used to determine Nicotine in dried and fresh mushrooms under basic conditions with primary secondary amino sorbent (PSA) clean up. The chromatography was performed on C 18 reversed phase column using a gradient of acetonitrile and ammonium formiate lmM pH = 3.4 as mobile phase at a flow rate of 0.3 mL min^-1. Nicotine was determined by using Nicotine-d3 as internal standard. Limit of quantification (LOQ) was 0.01 mg kg^-1 for both fresh and dried mushrooms. Calibration curve was linear over the concentration range of 0.01-2.3 mg mL^-1, with r2 〉 0.99. As for recoveries in dried mushrooms, spiking levels of 0.32 mg kg^-1 and 2 mg kg^-1 were considered whereas for the fresh mushrooms the recoveries were determined at 0.036 mg kg^-1 and 0.36 mg kg^-1. Satisfactory results were obtained for both matrices and the recoveries proved to range from 105% to 135%, with a standard deviation in the range 17-20. The method was applied to the analysis of Nicotine to assess the levels of nicotine in fresh and dried mushrooms.