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中国精品科技期刊2020
范小龙,朱正伟,吴婉琴,等. 植物油中叔丁基对苯二酚转化产物的识别确证与测定[J]. 食品工业科技,2022,43(11):303−309. doi: 10.13386/j.issn1002-0306.2021090133.
引用本文: 范小龙,朱正伟,吴婉琴,等. 植物油中叔丁基对苯二酚转化产物的识别确证与测定[J]. 食品工业科技,2022,43(11):303−309. doi: 10.13386/j.issn1002-0306.2021090133.
FAN Xiaolong, ZHU Zhengwei, WU Wanqin, et al. Identification, Confirmation and Determination of Tert-Butylhydroquinone Degradation Products in Vegetable Oil[J]. Science and Technology of Food Industry, 2022, 43(11): 303−309. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021090133.
Citation: FAN Xiaolong, ZHU Zhengwei, WU Wanqin, et al. Identification, Confirmation and Determination of Tert-Butylhydroquinone Degradation Products in Vegetable Oil[J]. Science and Technology of Food Industry, 2022, 43(11): 303−309. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021090133.

植物油中叔丁基对苯二酚转化产物的识别确证与测定

Identification, Confirmation and Determination of Tert-Butylhydroquinone Degradation Products in Vegetable Oil

  • 摘要: 目的:通过模拟日常生活中植物油加热的过程,确定了含有叔丁基对苯二酚(TBHQ)植物油样品中TBHQ转化降解的条件,采用气相色谱-质谱检测、未知化合物与数据库的匹配最终确定了TBHQ两种转化产物叔丁基对苯醌(TQ)、2,5-二叔丁基-1,4-苯醌(TBK),并建立了植物油中TBHQ及其两种降解产物TQ、TBK气相色谱-质谱联用检测方法。方法:样品经乙腈饱和的正己烷溶解,正己烷饱和的乙腈提取,取乙腈层,提取两次,合并乙腈层,40 ℃水浴下减压浓缩至近干,甲醇复溶,采用HP-5MS UI毛细管柱(30 m×0.25 mm,0.25 μm),不分流进样,选择离子监测模式,气相色谱-质谱仪测定,外标法定量。结果:3种化合物在各自浓度范围内线性良好(R2>0.995),在3个加标水平下,平均回收率范围为83.40%~107.71%,相对标准偏差(n=6)小于8.50%。3种化合物定量限TBHQ和TBK为10 μg/kg,TQ为50 μg/kg,25批次样品测定,其中两批次样品测定出TQ,该样品经加热处理后均测定出TBK。结论:该方法操作简便,灵敏度高,准确可靠,适用于植物油中TBHQ及其降解产物的同时测定。

     

    Abstract: Objective: By simulating the heating process of edible oil in daily life, the transformation and degradation conditions of tert butyl hydroquinone (TBHQ) in vegetable oil samples containing TBHQ were determined. The two transformation products of TBHQ, tert butyl p-benzoquinone (TQ) and 2,5-di-tert-butyl-1,4-benzoquinone (TBK), were finally determined by gas chromatography-mass spectrometry and matching of unknown compounds with the database. And a gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of tert-Butyl-hydroquinone (TBHQ) and its two degradation products 2-tert-Butyl-1,4-benzoquinone (TQ) and 2,5-di-tert-butyl-1,4-benzoquinone (TBK) in vegetableoil. Methods: The sample was dissolved in n-hexane saturated with acetonitrile and extracted with acetonitrile saturated with n-hexane. The acetonitrile layer was extracted twice, and the acetonitrile layer was combined. The acetonitrile layer was concentrated to nearly dry in 40 ℃ water bath and then redissolved with methanol, HP-5MS UI capillary column (30 m×0.25 mm, 0.25 μm) was used without splitter injection. Then selected the ion monitoring mode, gas chromatography-mass spectrometry determination, external standard method quantitative. Results: The linear range of the three compounds was good (R2>0.995). Under the three levels of concentration, the recoveries were 83.40%~107.71%, and the relative standard deviation (n=6) was less than 8.5%. The limits of quantitation (loqs) of TBHQ and TBK were 10 μg/kg and TQ was 50 μg/kg. 25 batches of samples were measured. TQ was measured in two batches of samples, and TBK was measured after heating treatment. Conclusion: The method is simple, sensitive, accurate and reliable. It is suitable for the simultaneous determination of TBHQ and its degradation products in vegetable oil.

     

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