加速溶剂萃取结合亲水液相色谱柱分离测定坚果中的8种生育酚异构体
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(浙江省疾病预防控制中心,浙江 杭州 310051)

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郑熠斌 男 初级技师 研究方向为食品理化检测技术的开发 E-mail:ybzheng@cdc.zj.cn通信作者:黄百芬 女 主任技师 研究方向为食品理化检测技术的开发 E-mail:bfhuang@cdc.zj.cn

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Simultaneous and quick determination of all eight vitamin E isomers in nuts by accelerated solvent extraction and hydrophilic interaction liquid chromatography
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(Zhejiang Provincial Centre for Disease Control and Prevention, Zhejiang Hangzhou 310051, China)

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    摘要:

    目的 建立加速溶剂萃取(ASE)结合亲水液相色谱(HILIC)柱分离测定坚果中8种生育酚异构体的方法。方法 2 g坚果样品经ASE提取富集后,用BEH Amide色谱柱(150 mm×3.0 mm, 1.7 μm)分离,以90%正己烷,10%叔丁基甲基醚-四氢呋喃-甲醇(20∶1∶0.1,V/V)作为流动相等度洗脱,荧光检测器激发波长294 nm,发射波长328 nm检测,外标法定量。结果 4种生育酚在0.5~80.0 μg/ml、4种生育三烯酚在0.5~30.0 μg/ml之间具有良好的线性(r2>0.998),方法检出限在0.032~0.070 mg/kg之间,方法定量限范围0.096~0.210 mg/kg,三个水平加标回收率在87.5%~114.2%之间,6次重复测定相对标准偏差(RSD)均≤12%。结论 本方法具有良好的灵敏度、回收率和重复性,适用于坚果中8种生育酚异构体的含量分布的测定。

    Abstract:

    Objective A method was developed for simultaneous quantification of eight E vitamers (tocopherols and tocotrienols with α, β, γ and δ type) in nut matrix by hydrophilic interaction liquid chromatography (HILIC) after pretreating with accelerated solvent extraction. Methods Nut samples were extracted using accelerated solvent extraction (ASE), the separation of 8 anlaytes was achieved using BEH amide amino column (150 mm×3.0 mm, 1.7 μm) and the mobile phase was 90% hexane and 10% methyl tert-butyl ether-tetrahydrofuran-methanol (20∶0.1, V/V). Results The detection limits were ranged from 0.032 to 0.070 mg/kg with linear correlation coefficient above 0.998, while quantification limits were 0.096-0.210 mg/kg. Intraday and interday recoveries of spiking standards were 87.5%-114.2%, and relative standard deviations (RSDs) were all less than 12%. Conclusion The established method could be applied in the simultaneous detection of vitamin E isomers in nuts due to its excellent sensitivity, recovery and reproducibility.

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郑熠斌,潘晓东,许娇娇,黄百芬.加速溶剂萃取结合亲水液相色谱柱分离测定坚果中的8种生育酚异构体[J].中国食品卫生杂志,2017,29(6):698-702.

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  • 收稿日期:2017-08-08
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  • 在线发布日期: 2018-01-29
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