摘要
研究了分子印迹固相萃取高效液相色谱法测定植物油中苯并(a)芘含量的方法关键点、加标回收率和精密度。方法关键点为确立荧光最优检测波长和选择无本底含量的试验试剂,可以提高方法的灵敏度和结果的准确性。苯并(a)芘的荧光最优激发波长为362 nm,发射波长为410 nm。试验试剂本身可能含苯并(a)芘,应优先选择同批次无本底含量的试验试剂。油茶籽油中低、中、高3个不同苯并(a)芘添加量的加标回收率分别为95.7%、94.5%和95.2%,植物油中低、中、高3个不同苯并(a)芘含量的测定结果相对标准偏差分别为1.4%、1.8%和2.1%。结果表明方法加标回收率高,精密度好。通过比较分子印迹柱和中性氧化铝柱净化效果,分子印迹柱的测定结果更加稳定,在实际检测应用中更有优势。将方法应用于植物油中苯并(a)芘测定能力验证,评价结果满意。
The key points of method, standard recovery rates and method precision of determine benzo (a)py- rene content in vegetable oils by high performance liquid chromatography with molecularly imprinted solid phase ex- traction were studied in this paper. The key points of method were to confirm optimal detection wavelength of fluores- cence detector and to choice experiment reagents with no background content. The optimal wavelength of fluorescence detector to determent benzo (a)pyrene content was the excitation wavelength of 362 nm and the emission wavelength of 410 nm. The experiment reagents might contain benzo(a)pyrene themselves, and gave priority to use of the same batch of reagents with non benzo(a) pyrene. The standard recovery rates of adding benzo(a) pyrene standard on low, medium and high concentration in camellia seed oil were 95.7% , 94.5% and 95.2% respectively, and the relative standard deviation (RSD) of method on low, medium and high concentration for benzo (a) pyrene in vegetable oils were 1.4% , 1.8% and 2.1% respectively. The results indicated that the method had high standard recovery rates and good precision. Through the comparison between the method of molecularly imprinted column purification and the method of neutral alumina column purification, the method of molecularly imprinted column purification was more sta- ble and had greater application advantage. The evaluation of proficiency testing benzo (a) pyrene content in vegetable oils received good results.
出处
《中国粮油学报》
EI
CAS
CSCD
北大核心
2017年第7期127-132,共6页
Journal of the Chinese Cereals and Oils Association
关键词
苯并(A)芘
分子印迹
固相萃取
高效液相色谱法
荧光检测
Benzo(a) pyrene, molecularly imprinted technology, solid phase extraction, high performance liq-uid chromatography, fluorescence detection