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摘要
An alternative method based on an off-line solid phase extraction (SPE) combined with programmable temperature vaporizer-based (PTV) large volume injection-gas chromatography-flame ionization detection (LVI-GC-FID) was developed. The goal of this study was to determine mineral oil saturated hydrocarbons (MOSH) in camellia seed oils. The purification condition of SPE columns with silver impregnated the activated silica gel and activated aluminum oxide was optimized. The optimal SPE cartridge was loaded with 10 g of Ag-activated silica gel per 10 g of activated aluminum oxide. The PTV initial temperature was set at 75 degrees C for 1 min (split 200:1), and heated from 75 degrees C to 370 degrees C at 250 degrees C/min. Then the diverter valve was closed for 1 min and opened again with the split flow ratio changing to 50:1. The injection volume was 40 mu L. The calibration curve of paraffin oil was liner in the range of 5-500 mg/kg with correlation coefficient of 0. 998. The detection limit (LOD) and the quantification limit (LOQ) of paraffin oils in hexane were 0. 26 mg/kg and 0. 80 mg/kg, respectively. The recoveries from spiked oil samples were between 93. 3% and 112. 7%, with relative standard deviation (RSD) of 1. 8%-5. 2%, the RSD of intra. day and inter. day were less than 2. 6%. This procedure was applied to analyze the MOSH in 11 commercial camellia seed oils and the contamination was found to range from 6. 8 mg/kg to 76. 7 mg/kg. The method is simple in operation with high sensitivity, good reproducibility and low cost, and suitable for determination of MOSH in vegetable oils.
- 出版日期2016-9
- 单位北京市理化分析测试中心; 北京化工大学
