Determination of 5 Phenyl Ethyl Carboxylates in Cut Tobacco by GC-MS/MS with Accelerated Solvent Extraction and Evaluation on Uniformity Evalution of the Aromatizing Process

Cut tobacco sample was equilibrated for 24 h under the condition of (20±1)℃ and relative humidity of (60±3)%. A portion (4.0 g) of the equilibrated sample was taken and transferred to the 34 mL of extraction cell of the Dionex ASE 350 extractor and submitted to ASE with n-hexane. In ASE process, conditions of temperature (100℃), static extraction time (5 min), and cycling frequency (2 times) were adopted. The extract was separated and 0.50 mL of 100 mg·L^-1 phenylmethyl acetate solution was added as internal standard. After well mixing and filtration through 0.45 μm filtering membrane, the filtrate was used for GC-MS/MS analysis. Chromatographic separation was carried out on HP-5MS capillary column (30 m×0.25 mm, 0.25 μm) and under the mode of programmed temperature elevation ranged from 60℃ to 280℃. EI and MRM mode were used in MS/MS determination. Linearily ranges of standard curves of the 5 phenylethyl carboxylates determined were found same between 0.10 mg·L^-1 and 10.00 mg·L^-1, and their detection limits (3S/N) were found having the same value of 0.01 mg·L^-1. Recovery was tested by standard addition method, and the results of recovery were found in the range of 91.0%-107%, and values of RSDs (n=6) were found all less than 10%. Uniformity of aromatizing process for the cut tobacco were tested on samples taken from intra and inter production batches of the aromatizing process, giving values of coefficients of variation (CV_i) in the ranges of 5.8%-8.8% and 6.3%-8.4%, respectively, showing that the uniformity of aromatizing was good and satifactory.