RP-HPLC法测定植物油中苯并(a)芘残留量

Determination of the Benzo(α)pyrene in Vegetable Oil by RP-HPLC

建立RP-HPLC法测定植物油中苯并(a)芘残留量的方法。采用Thermo Acclaim^TM 120 C18色谱柱(250mm×4.6 mm, 5.0μm),以乙腈-水(90︰10, V/V)溶液为流动相进行洗脱,流速1.0 mL/min,柱温35℃,荧光检测器检测(激发波长384 nm,发射波长406 nm)。结果表明,苯并(a)芘线性范围为0~19.76 ng/mL (r=0.999 9);平均回收率(n=9)为100.25%(加标浓度0.2, 0.4和0.6μg/kg);检出限为2.08×10-3μg/kg;供试品溶液在24 h内稳定, RSD (n=6)为0.41%;方法耐用性好,在不同柱温(±1℃)条件下, RSD (n=3)为0.58%,不同流速(±0.1 mL/min)条件下, RSD(n=3)为0.71%。20批试样中苯并(a)芘含量为0.214 7~2.883 6μg/kg。该方法经方法学验证,适用于苯并(a)芘的品质控制。

To establish an RP-HPLC method for determining the benzo(α) pyrene in vegetable oil. The analysis was performed on an Thermo Acclaim^TM 120 C18 column(250 mm×4.6 mm, 5.0 μm) with gradient elution of acetonitrile and water(90︰10, V/V) at the flow rate of 1.0 mL/min. The column temperature was 35 ℃, and the benzo(α) pyrene was detected with FLD(Ex of 384 nm, Em of 406 nm). Results showed that the liner range of calibration curve was 0-19.76 ng/mL(r=0.999 9), and the average recovery(n=9) was 100.25%(standard additive concentration 0.2, 0.4 and 0.6 μg/kg). The limit of detection was 2.08×10-3 μg/kg. The sample solution was stable within 24 h, and the RSD(n=6) was 0.41%. The robustness was investigated by varying the conditions of column temperature(±1 ℃) and flow rate(±0.1 mL/min), with the RSD of 0.58% and 0.71%. The contents of the benzo(α) pyrene in twenty samples were 0.214 7-2.883 6 μg/kg. The established method was validated to be suitable for quality control of the benzo(α) pyrene.