Citation: LI Bing-Ning, LIU Ling-Ling, ZHANG Zhen-Xia, WU Yan-Wen. Ag-Solid-Phase Extraction-Programmed Temperature Vaporization- Gas Chromatography for Analysis of Mineral Oil-Saturated Hydrocarbons in Commercial Chocolates[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(4): 514-520. doi: 10.11895/j.issn.0253-3820.160828 shu

Ag-Solid-Phase Extraction-Programmed Temperature Vaporization- Gas Chromatography for Analysis of Mineral Oil-Saturated Hydrocarbons in Commercial Chocolates

1.
Beijing Center for 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.
Xi'an Communication institute, Xi'an 710106, China

Received Date: 14 November 2016
Revised Date: 12 January 2017

An offline silver-impregnated silica gel solid-phase extraction (Ag-SPE) approach combined with a programmed temperature vaporization-gas chromatography-flame ionization detector (PTV-GC-FID) was proposed for routine analysis of mineral oil saturated hydrocarbons (MOSH) in chocolates. The MOSH in chocolates were extracted by n-hexane and 1 mL of extract was purified by offline Ag-SPE column. The SPE columns packed with 0.3% Ag-activated silica gel were used to separate MOSH from triglycerides and olefins in chocolates. The eluent of MOSH fraction was only 5 mL and then concentrated to 0.2 mL through nitrogen blowing with little evaporation loss. The PTV parameters were as follows: the initial temperature was set at 45℃ and held for 1 min (split ratio was 200:1), then warmed up to 360℃ at linear gradient of 250℃ min^-1 and held for 27 min (split valve was closed for 2 min followed by split ratio of 100:1). The GC injection volume was 40 μL. The GC column was heated from 35℃ (3 min) to 350℃ at 25℃/min, and then raised to 370℃ (10 min) at 5℃/min. The flow rate of the carrier gas was 1.3 mL/min (and pressure was 60 kPa), FID temperature was set at 380℃. The limit of quantification (LOQ) and the recoveries of the method were 0.5 mg/kg and 84.9%-108.6%, respectively, with the relative standard deviations (RSD) of 0.2%-1.5%. Twenty-five commercial chocolate samples were analyzed with the proposed method, and it was found that the MOSH in three samples were not detected, and the concentrations of MOSH in other 22 samples were 1.09-8.15 mg/kg (the concentrations of MOSH with C₁₆-C₃₅ component were 0.56-4.43 mg/kg). The results suggested that it was necessary to routinely detect mineral oil contamination in chocolates for food safety.
- Chocolate,
- Mineral oil contamination,
- Saturated hydrocarbons,
- Solid phase extraction,
- Gas chromatography,
- Hydrogen flame ionization detector
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沈阳化工大学材料科学与工程学院沈阳 110142