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Citation: LIU Ling-Ling, WU Yan-Wen, LI Bing-Ning, WANG Yu, YANG Yi-Fan, ZU Wen-Chuan, WANG Xin-Xin. An Off-line Solid Phase Extraction Combined with Large Volume Injection-Gas Chromatography-Flame Ionization Detection Method for Determination of Mineral Oil Saturated Hydrocarbons in Camellia Seed Oils[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(9): 1419-1424. doi: 10.11895/j.issn.0253-3820.160138 shu

An Off-line Solid Phase Extraction Combined with Large Volume Injection-Gas Chromatography-Flame Ionization Detection Method for Determination of Mineral Oil Saturated Hydrocarbons in Camellia Seed Oils

1.
Beijing Center of Physical and Chemical Analysis, Beijing Food Safety Analysis and Testing Engineering Research Center, Key Laboratory of Analysis and Testing, Beijing Academy of Science and Technology, Beijing 100089, China
2.
Analysis and Testing Center, College of Science, Beijing University of Chemical Technology, Beijing 100029, China

Received Date: 29 February 2016
Revised Date: 31 May 2016

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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℃ for 1 min (split 200:1), and heated from 75℃ to 370℃ at 250℃/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 μL. 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.
- Camellia seed oils,
- Mineral oil saturated hydrocarbons,
- Solid phase extraction,
- Large volume injection-gas chromatography,
- Aluminum oxide
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