皂化提取-高效液相色谱法测定油茶籽油中苯并(a)芘残留

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

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2.00～20.0μg/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0.2μg/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。

An analytical method was developed for determination of benzo（a） pyrene in oil -tea camellia seed oil by saponification with 2 mol/L KOH - CH3 CH2OH 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℃ o At fortification levels of 2.00 - 20.0μg/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.