皂化提取-高效液相色谱荧光法测定油炸食品中5种多环芳烃

Determination of five kinds of PAHs in fried foods by HPLC- FLD after saponification extraction

建立了皂化提取-高效液相色谱荧光法测定油炸食品中苯并（a）芘、苯并（a）蒽、苯并（b）荧蒽、苯并（k）荧蒽及苯并[g,h,i]苝等5种多环芳烃的检测方法。油炸食品样品经皂化法处理,用正己烷提取,经浓缩处理后,用乙腈溶解,经高效液相色谱荧光定量检测。分离柱为Waters PAH C18柱（250 mm×4.6 mm i.d.,5μm）;流动相为水-乙腈体系,梯度洗脱;流速1.0 mL/min,检测波长：苯并（a）蒽：λex=290 nm,λem=400 nm;其它4种目标物：λex=290 nm,λem=430 nm。不同基质样品中5种多环芳烃的定量限为0.1-0.6μg/kg。不同基质样品中5种多环芳烃的回收率为84.7%-106.3%,RSD为1.1%-3.2%（n=6）,在相应浓度范围内呈良好的线性关系,线性相关系数均大于0.999。

A method was developed to determine five kinds of PAHs including benzo （a） pyrene, benz （a） anthracene, benzo（b） fluoranthene, benzo（k） fluorathene and 1,12-benzoperylene in fried foods by HPLC - FLD after saponification extraction. The samples were extracted with hexane after saponified and hexane was concentrated by rotary evaporator, then the residual was dissolved by acetonitrile. After the chromatographic separation on a Waters PAH C18（5 μm,250 mm ×4. 6 mm） column by gradient elution with water-acetonitrile was performed, the analysis was carried out by HPLC - FLD. The rate of mobile phase was 1.0 mL/min. The λem was 290 nm for five kind of PAHs and the λem were 400nm for benz（a） anthracene and 430nm for other PAHs. The correlation coefficients of determination of PAH in the fried foods were more than 0. 999. The recoveries were ranged from 84. 7% to 106. 3%, and the relative standard deviations were 1.1% ~ 3.2% （n = 6）. The results indicated the method was convenient, stable, reliable and special for the determination of PAHs in fried foods.