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浙江大学学报（农业与生命科学版）
浙江大学学报(农业与生命科学版)  2015, Vol. 41 Issue (2): 189-194    DOI: 10.3785/j.issn.1008-9209.2014.09.091
食品科学     
固相萃取超高效液相色谱荧光法检测植物油中苯并［a］芘
冯寅洁1, 乔勇升1, 陈伟1, 冯成玉2, 应铁进3
1.江苏省泰州市食品药品检验所，江苏 泰州 225300；2.江苏省海安县农业委员会，江苏 海安 226600；3.浙江大学生物系统工程与食品科学学院食品科学与营养系，杭州 310058
Determination of benzo ［a］ pyrene in vegetable oil by solid phase extraction-ultra performance liquid chromatography-fluorescence detector.
Feng Yinjie1, Qiao Yongsheng1, Chen Wei1, Feng Chengyu2, Ying Tiejin3
(1. Taizhou Institute for Food and Drug Control, Taizhou 225300, Jiangsu, China; 2. Agricultural Commission of Hai’an County, Hai’an 226600, Jiangsu, China; 3. Department of Food Science & Nutrition, School of Biosystems Engineering and Food Science, Zhejiang University, Hangzhou 310058, China)
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摘要： 为建立固相萃取超高效液相色谱大体积流通池荧光法检测植物油中苯并［a］芘（benzo ［a］ pyrene, BaP）的方法，对4种商业化固相萃取柱净化油样和富集BaP的效果进行评价，同时比较了4种超高效液相色谱柱的分离效果。结果表明：借助商业化BaP专用固相萃取柱处理样品，洗脱液旋蒸至干后用乙腈四氢呋喃(体积比为9∶1)溶解定容，经过BEH Shield RP18柱（50 mm×2.1 mm, 1.7 μm）分离，流动相为乙腈水(体积比为70∶30)，流速0.4 mL/min，BaP在0.101~10.1 μg/L范围内有良好的线性关系（r>0.999 993），检出限为0.2 μg/kg；商业化固相萃取柱能较好地除去样品中的油和吸附BaP，4种固相萃取柱的3个加标水平的回收率为91.0%~106.9%，相对标准偏差为1.4%~9.6% (n=6)；用超高效液相色谱法分析样品，速度比高效液相色谱快3倍。与国标相比，该方法具有操作简便、重复性好、灵敏度高、节省溶剂等优越性，可快速、准确地对植物油中的BaP进行定性和定量检测。
Abstract: Benzo ［a］ pyrene (BaP) is a kind of polycyclic aromatic hydrocarbon, which is recognized as one of the three major carcinogens found in foods. The source of BaP detected in vegetable oil are as follows: BaP may occur when oilseeds are dried, smoked and stir-fried; organic solvents used in the leaching process may have polycyclic aromatic hydrocarbons; oil heated over temperature or overtime in the process of production and cooking may produce BaP. The recommended national method for BaP determination in animal and vegetable fats and oils (GB/T 22509—2008) requires high experimental skills and long test time, making it difficult to guarantee the accuracy and repeatability of results. Besides, another standard on determination of BaP in foods (GB/T 5009.27—2003) is also complicated in sample pretreatment. In this study, a method for the determination of BaP in vegetable oil by solid phase extraction-ultra performance liquid chromatography-fluorescence detector (SPE-UPLC-FLD) with a large volume flow cell was established. Oil samples were purified by four kinds of commercial solid phase extraction cartridges to compare extraction effects. Besides, the four types of chromatographic columns used in UPLC were tested to analyze separation effects. Samples were cleaned and enriched by commercial solid phase extraction cartridges. Then, the elution was dried by rotary evaporation and then was dissolved with acetonitrile-tetrahydrofuran (volume ratio, 9∶1) to a constant volume. Sample solution was separated by BEH Shield RP18 column (50 mm×2.1 mm, 1.7 μm) with the mobile phase of acetonitrile-water (volume ratio, 70∶30) at the flow rate of 0.4 mL/min. Results showed that under the optimized conditions, a good linear relationship (r>0.999 993) was obtained in the range of 0.10110.1 μg/L Bap, with detection limit of 0.2 μg/kg. Recovery rates for four kinds of solid phase extraction cartridges were 91.0%106.9% in three spike levels, and relative standard deviations (RSD) were 1.4%9.6% (n=6). Sample analysis by UPLC was three times faster than HPLC. In conclusion, this method has many advantages such as simple pretreatment, good repeatability, high sensitivity, less solvent and so on, thus can be applied on the rapid qualitative analysis and accurate quantitative detection of BaP in vegetable oil.
出版日期: 2015-03-20
CLC:  TS 227  
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冯寅洁
乔勇升
陈伟
冯成玉
应铁进

引用本文:

冯寅洁, 乔勇升, 陈伟, 冯成玉, 应铁进. 固相萃取超高效液相色谱荧光法检测植物油中苯并［a］芘[J]. 浙江大学学报(农业与生命科学版), 2015, 41(2): 189-194.

Feng Yinjie, Qiao Yongsheng, Chen Wei, Feng Chengyu, Ying Tiejin. Determination of benzo ［a］ pyrene in vegetable oil by solid phase extraction-ultra performance liquid chromatography-fluorescence detector.. Journal of Zhejiang University (Agriculture and Life Sciences), 2015, 41(2): 189-194.

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http://www.zjujournals.com/agr/CN/10.3785/j.issn.1008-9209.2014.09.091    或    http://www.zjujournals.com/agr/CN/Y2015/V41/I2/189

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