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

作　　者：汤富彬[1] 莫润宏[1] 钟冬莲[1] 沈丹玉[1] 费学谦[1] 倪张林[1] 屈明华[1] 

机构地区：[1]中国林业科学研究院亚热带林业研究所,国家林业局经济林产品质量检验检测中心,浙江富阳311400

出　　处：《中国油脂》2012年第2期62-64,共3页China Oils and Fats

基　　金：中央级公益性科研院所基本科研业务费专项资金(RISF6149,RISF6151);国家科技支撑计划(2009BADB1B09)

摘　　要：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.

关 键 词：苯并(A)芘 油茶籽油 皂化提取 高效液相色谱法 

分 类 号：TS227[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.72[轻工技术与工程—食品科学与工程]