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.
出处
《职业与健康》
CAS
2015年第4期456-458,共3页
Occupation and Health
关键词
苯并[A]芘
油炸面制品
高效液相色谱荧光检测
Benzo（a） pyrene
Fried dough foods
High performance liquid chromatography with fluorescence detection
