A rapid, sensitive and solvent-less method for determination of malonaldehyde in meat by stir bar sorptive extraction coupled thermal desorption and gas chromatography/mass spectrometry with in situ derivatization.
BACKGROUND
The traditional methods for analysis of malonaldehyde (MDA), such as the thiobarbituric acid (TBA) assay, require strong acidity at high temperature for derivatization and lack specificity in analysis. Stir bar sorptive extraction (SBSE) coupled with thermal desorption-gas chromatography/mass spectrometry (TD-GC/MS) with in situ derivatization using pentafluorophenylhydrazine (PFPH) under mild conditions is an emerging technique for MDA analysis.


METHODS
MDA in meat was derivatized with PFPH at pH ~4 for 1 h at room temperature, forming a relative stable derivative of MDA-PFPH. The derivative of MDA-PFPH was simultaneously extracted using SBSE. Then, MDA-PFPH was thermally released and quantitatively analyzed by GC/MS in selected ion monitoring (SIM) mode.


RESULTS
The method of SBSE-TD-GC/MS for MDA analysis with in situ derivatization was optimized and validated with good linearity, specificity and limit of detection/quantification (LOD/LOQ). The method was successfully applied for analysis of MDA in raw and cooked meat (pork).


CONCLUSIONS
The SBSE-TD-GC/MS method was suitable to monitor and analyze MDA in meat samples at trace levels. The simple, sensitive and solvent-less method with moderated in situ derivatization can be applied for analysis of MDA in a wide variety of foods and biological samples.
Lacombe Research Centre, Agriculture and Agri-Food Canada, 6000 C&E Trail, Lacombe, AB T4L 1W1, Canada; State Key Laboratory of Environmental and Biological Analysis, Chemistry Department, Hong Kong Baptist University, 224 Waterloo Road, Kowloon, Hong Kong SAR, China.
Eric Dongliang
ED
Ruan
Jennifer
J
Aalhus
Manuel
M
Juárez
D000818:Animals; D005591:Chemical Fractionation / Q000379:methods*; D003296:Cooking; D005504:Food Analysis / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006834:Hydrazines; D057230:Limit of Detection; D016014:Linear Models; D008315:Malondialdehyde / Q000032:analysis*; D008460:Meat / Q000032:analysis*; D015203:Reproducibility of Results; D013552:Swine; D005464:Fluorobenzenes; D005466:Fluorocarbons
D006834:Hydrazines; D008315:Malondialdehyde; C031120:(pentafluorophenyl)hydrazine; D005464:Fluorobenzenes; D005466:Fluorocarbons