基于HiCapt Benzo固相萃取前处理的HPLC-FLD法检测油茶籽油中苯并(a)芘

A detection method over benzo(a) pyrene in Camellia oleifera Abel seed oil by HPLC-FLD based on Hi Capt Benzo solid-phase extraction pretreatment

为了建立一种基于Hi Capt Benzo固相萃取快速前处理的,更灵敏、准确的高效液相色谱-荧光检测法,以用于油茶籽油中苯并(a)芘的检测。油茶籽油样品以正己烷溶解后,用Hi Capt Benzo专用固相萃取柱净化。检测条件为:LC-PAHs专用色谱柱;50%乙腈-50%水为流动相,流速1.0 m L/min;荧光检测器;外标法定量。研究结果表明,苯并(a)芘标准曲线在0.1~200 ng/m L范围内,线性关系好(R^2=0.9993);检测限很低(0.0213~0.0246μg/kg)。该法用于4个油茶籽油样品加标检测,回收率为93.06%~104.52%,相对标准偏差(RSD)为2.12%~3.98%。本文所建固相萃取-高效液相色谱(带荧光检测器)法前处理简单,结果准确可靠,是油茶籽油苯并(a)芘高效检测的适宜方法。

This study was aimed to establish a highly efficient method of high-performance liquid chromatography with fluorescence detection（HPLC-FLD） based on Hi Capt Benzo solid-phase extraction time-saving pretreatment for benzo（a） pyrene [B（a）P] detection in Camellia oleifera Abel seed oil（COASO）. Samples of COASO were dissolved in hexane,and purified by Hi Capt Benzo solid phase extraction（SPE） column. The detection conditions were as followings：LC-PAHs chromatographic column,50% acetonitrile-50% pure water as mobile phase,flow rate 1.0 m L/min,fluorescence detector,quantification by external standard method. The results showed that standard calibration curve was linear over the concentration range of 0.1~200 ng/m L,with the regression efficiency（R^2） of 0.9993. Furthermore,the detection limit was 0.0213~0.0246 μg/kg. A recovery range of 93.06%~104.52%and a relative standard deviation（RSD） range of 2.12%~3.98% was exhibited when the method was employed to detect four samples of COASO added with [B（a）P] standand. It was suggested that this detection method of SPE-HPLC-FLD established in the study was a suitable one for [B（a）P] detection in COASO,for its obvious advantages,such as simpler pretreatment,more sensitive and more efficient.