Direct measurement of 3-chloropropane-1,2-diol fatty acid esters in oils and fats by HPLC method

A new high performance liquid chromatography (HPLC) method for the measurement of 3-chloropropane-1,2-diol fatty acid esters in oil samples without any derivatization treatment is presented in this paper. The qualification analysis of 3-MCPD esters was performed by UPLC-Q-TOF MS while quantification analysis was carried out by HPLC method using 1,2-dioleoyl-3-chloropropanediol and 1-stearoyl-3-chloropropanediol standards as reference standard substances. The linearity was verified (correlation coefficients > 0.99) within the concentrations ranged from 0.01 to 0.28 mg mL−1. The intraday precision ranged from 2.1 to 4.0%, and the interday precision ranged between 3.2 and 5.6%. The recovery values of 3-MCPD esters standard substances spiked canola oil sample at the concentrations of 800, 1000 and 1200 mg kg−1 were found to be 106.6% ± 11.8, 94.7% ± 13.3 and 105.8% ± 8.8 for 1,2-dioleoyl-3-chloropropanediol, 91.9% ± 12.3, 87.5% ± 5.3 and 108.6% ± 3.7 for 1-stearoyl-3-chloropropanediol, respectively. The limit of detection (LOD) and limit of quantification (LOQ) were 3.43 and 5.71 μg mL−1 for 1,2-dioleoyl-3-chloropropanediol, 2.55 and 5.66 μg mL−1 for 1-stearoyl-3-chloropropanediol, separately.