皂化提取－高效液相色谱法测定油茶籽油中苯并(a)芘残留

建立了一种先皂化油茶籽油,经萃取和净化,高效液相色谱-荧光检测器测定油茶籽油中苯并(a)芘的检测方法.采用2 mol/L氢氧化钾乙醇溶液皂化,石油醚萃取,中性氧化铝净化柱净化后,再在下述条件下测定:多环芳烃(PAH)C18柱,流动相为体积比95∶5的乙腈-0.5％磷酸水溶液,流速1.0 mL/min,荧光激发波长384 nm,发射波长406 nm,柱温30℃.在2.00 ～ 20.0 μg/kg的添加水平,加标回收率在93.0％～110.0％之间,相对标准偏差在2.59％～9.57％,该方法的检出限为0.2 μg/kg.该方法对油茶籽油中苯并(a)芘提取完全,操作简单,重现性好,检测灵敏度高,对阳性样品判断更有优势.

Saponification-extraction and HPLC determination of benzo(a) pyrenein oil-tea camellia seed oil

An analytical method was developed for determination of benzo(a)pyrene in oil-tea camellia seed oil by saponification with 2 mol/L KOH-CH3CH2OH solution and extraction with petroleum ether,and then purification by a neutral aluminium column,then determination with HPLC.The determination conditions were as follows: analysis cloumn PAH C18,mobile phase acetonitrile/water(containing 0.5%phosphoric acid)95∶5,flow rate 1.0 mL/min,excitation wavelength 384 nm,emission wavelength 406 nm,column temperature 30 ℃.At fortification levels of 2.00～20.0 μg/kg,recoveries for benzo(a)pyrene varied from 93.0% to 110.0%,the relative standard deviation varied from 2.59% to 9.57%,the limit of detection was 0.2 μg/kg.The method was characterized by simplicity,sensitivity and accuracy.