油炸面制品中的苯并[a]芘的高效液相色谱荧光测定法  

Determination of benzo (a) pyrene in fried dough foods by high performance liquid chromatography with fluorescence detection

作　　者：刘晓辉[1] 陈艳[1] 李永波[1] 何丰瑞 

机构地区：[1]陕西省西安市疾病预防控制中心,710054

出　　处：《职业与健康》2015年第4期456-458,共3页Occupation and Health

摘　　要：目的建立索氏提取法-SPE净化-高效液相色谱仪-荧光检测器检测油炸面制品中苯并[a]芘及多环芳烃的检测方法。方法油炸面制品经过粉碎,用正己烷经索氏提取器提取样品中的油脂,用中性氧化铝固相萃取柱净化提取油脂中的苯并[a]芘,净化后的样品处理液用Waters PHA 4.6×250mm色谱柱分离,为了达到良好的分离效果,使用乙腈：水梯度洗脱,流速1.5 ml/min,柱温30℃。在不同时间改变荧光检测器的激发波长及发射波长,提高检出限,用外标法定量。结果苯并[a]芘在0.01~0.5μg/ml范围内线性关系良好,r=0.999 2,检出限0.014μg/kg,加标回收率为74.7%~86.2%,测定了2013年西安市市售油炸制品中苯并[a]芘的含量为0.027~54.64μg/kg。结论该方法检出限低,灵敏度高,简便易于操作,适用于油炸面制品中苯并[a]芘的测定。[Objective]To establish a Soxhlet extraction-SPE purification-high performance liquid chromatograph-fluorescence detection method for benzo （a） pyrene and polycyclie aromatic hydrocarbon in fried dough foods.[Methods]The oil in fried dough foods were extracted with n-hexane by Soxhlet extraction, the benzo （a） pyrene in oil were extracted and purified with neutral alumina solid-phase extraction column, the purified liquid samples were separated on a Waters PHA （4.6×250 mm） special column. For getting good separation effect, the acetonitrile：water was used as the mobile phase at flow rate of 1.5 ml/min, with the column temperature at 30 ~C. The excitation wavelength and emission wavelength of fluorescence detector were changed at different time, to improve the detection limit. The quantitative analysis was carried out by external standard. [Results]The calibration curves were linear in the range of 0.01-0.5 μg/ml, r=0.999 2, the detectable limit was 0.014 μg/kg, and the recovery of standard addition was 74.7%-86.2%. The concentrations of benzo （a） pyrene in fried dough foods of Xi＇an City in 2013 were between 0.027 μg/kg and 54.64 μg/kg.[Conclusion]The method has the advantages of low detectable limit, high sensitivity and easy operation, aand it is suitable for the determination of benzo （a） pyrene in fried dough foods.

关 键 词：苯并[A]芘 油炸面制品 高效液相色谱荧光检测 

分 类 号：R115[医药卫生—公共卫生与预防医学]