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建立测定肉制品、动植物油脂中苯并(α)芘[B(α)P]含量的MAE-RHPLC法。样品经微波辅助萃取技术(MAE)富集、提取、净化,Agilent Eclipse XDB-C18柱(4.6 mm×250 mm,5μm)分离,流速1.0 mL/min的流动相(V(乙腈)︰V(水)=88︰12)洗脱,荧光检测器(λ发射:410 nm,λ激发:365 nm,狭缝:10 nm)检测,最后以峰面积外标法定量。B(α)P的检出限为0.01μg/kg,标准曲线线性范围为0μg/mL~42μg/mL,相关系数为0.999 9,方法回收率为97%~105%,精密度良好:日内RSD<1%、日间RSD<2%,准确度良好:测定值在甲醇中苯并(α)芘成分分析国家标准物质(GBW 08702)的标准值范围内。该法前处理简捷、高效、重现性好、回收率高,检出限、线性范围、准确度、精密度均满足要求,可用于大批量处理并测定肉制品、动植物油脂中B(α)P含量,也可参照用于处理、测定其它食品中B(α)P含量。
A MAE-RHPLC method for the determination of benzo (α) pyrene [B (α) P] content in meat products, animal and plant oils was established. The sample was concentrated by microwave assisted extraction (MAE), extracted, purified and separated on an Agilent Eclipse XDB-C18 column (4.6 mm × 250 mm, 5 μm) with a flow rate of 1.0 mL / min ) = 88: 12), detected by a fluorescence detector (λ emission: 410 nm, λ excitation: 365 nm, slit: 10 nm) and finally quantified by the peak area external standard method. The detection limit of B (α) P was 0.01μg / kg, the calibration curve linear range was 0μg / mL ~ 42μg / mL, the correlation coefficient was 0.999 9, the recovery was 97% ~ 105% <1%, daytime RSD <2% with good accuracy: the values are within the standard values of the national standard substance for benzo (a) pyrene analysis in methanol (GBW 08702). The pretreatment method is simple, efficient, reproducible, high recovery rate, the detection limit, linear range, accuracy and precision meet the requirements, can be used for large batch processing and determination of meat, animal and vegetable oils B (α ) P content, but also for reference for processing, determination of other foods B (α) P content.