Comparison of HPLC-FLD with GC-MS in Estimation of Benzo[a]pyrene in Sesame Oil
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Abstract:
The high-performance liquid chromatography-fluorescence detector (HPLC-FLD) method was optimized to determine benzo[a]pyrene (BaP) in sesame oil, and its applicability was compared with that of gas chromatography-mass spectrometry (GC-MS) with regard to methodology. Based on the Chinese standard method, GB/T 22509-2008, liquid–liquid extraction and neutral alumina column purification were used for pretreatment. Compared with GB/T 22509-2008, gradient elution was used in the HPLC-FLD method. Chromatographic conditions for GC-MS were as follows: column, HP-5MS capillary column (30 m × 0.25 mm × 0.25 μm); temperature program, gradient; injection port and transfer line temperature, 280 ℃; injection mode, pulsed splitless mode; carrier gas ?ow rate, 1.2 mL/min. The MS conditions were as follows: ionization mode, electron ionization (EI); temperature of ionization source, 230°C; quadrupole temperature, 150 ℃; with single ion monitoring (SIM) mode for quantitative analysis. The linear equations, limits of detection (LODs), recovery rates, and corresponding relative standard deviation(RSDs) for HPLC-FLD and GC-MS methods were Y = 817883X + 39074 (R2 = 0.9999) and Y = 1771.9X - 636.6 (R2 = 0.9997), 0.037 and 0.062 μg/kg, 82.40%~96.21% and 76.21%~94.19%, and 3.72%~6.64% and 5.18%~7.84%, respectively. For the same sesame oil sample, the BaP content determined by HPLC-FLD was higher than that determined by GB/T 22509-2008 and was significantly higher than that determined by GC-MS (P < 0.05). The results showed that both methods met the requirements for determination of BaP content in edible oils and fats. The HPLC-FLD method was better compared with GB/T 22509-2008 and its accuracy was greater than that of GC-MS.
