为了准确、快速检测食用油中苯并(a)芘的含量,建立了食用油中苯并(a)芘的超声波辅助一绿色溶剂萃取及GC/MS联用技术检测方法,其检出限和定量限分别为0.017肛g/L和0.053μg/L,加标回收率大于95%,日内和日间相对标准偏差分别为1.32%~1.76%和2.46%~3.17%,表明该方法符合痕量分析要求。实验考察了萃取剂种类、配比、用量、超声波功率、温度和时间对苯并(a)芘萃取的影响,获得了较优的萃取工艺条件:ACN—DMC配比(V/V)7:3,萃取剂用量25mL,超声功率300W,温度20℃,时间10min/次,萃取两次。采用该方法测定38个食用油样中苯并(a)芘含量,结果表明,其中30个不同品牌的新鲜食用油苯并(a)芘含量范围为0.09~8.17μg/kg;8个油炸食用油苯并(a)芘含量范围为6.03~11.73μg/kg。本方法耗时短且减少了有毒溶剂的使用,为食用油中含有的苯并(a)芘分析检测提供了一种科学简捷的方法。
Abstract: To quickly and accurately analyze B (a)p in edible oils, an ultrasonic assisted extraction with environmental friendly solvent using gas chromatography-mass spectrometry (GC-MS)method was developed. The limits of detection and quantization obtained were 0. 017 p,g/L and 0. 053μg/L respectively, and the recovery rate was higher than 95% and the relative standard deviations were 1.32% ~ 1.76% for inter-day and 2. 46% -3.17% for intra-day, demonstrating the proposed method was feasible and effective. Optimizing the conditions of ultrasound assisted extraction such as extractant, ration, dosage, ultrasonic power, temperature and time, an optimum method was deve- loped. The levels of B(a) p by using this method ranged from 0. 09 μg/kg to 8. 17μg/kg in 30 flesh edible oil samples, from 6.03 μg/kg to 11.73 μg/kg in 8 frying oil samples. The development of this method provided a scientific and simple method for determination of B (a) p in less time and solvent.