摘要
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.
作者
邹沫君
ZOU Mojun(Leshan Center for Food and Drug Control,Leshan 614000)
出处
《食品工业》
CAS
北大核心
2019年第12期268-270,共3页
The Food Industry