快速溶剂萃取—高效液相色谱—电感耦合等离子体质谱法测定富硒食用油中8种硒形态
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1.广州检验检测认证集团有限公司,广东 广州 511447;2.国家加工食品质量检验检测中心(广东), 广东 广州 511447;3.厦门医学院,福建 厦门 361023

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通讯作者:

梁志森(1989—),男,广州检验检测认证集团有限公司高级工程师,博士。E-mail: 522794556@qq.com
张书迪(1991—),男,厦门医学院副教授,博士。E-mail: zsd@xmmc.edu.cn

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基金项目:

福建省自然科学基金(编号:2022J05321);广东省市场监督管理局科技项目(编号:2023CZ07)


Determination of eight selenium species in selenium-enriched edible oil with accelerated solvent extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometry
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1.Guangzhou Inspection and Testing Certification Group Company Limited, Guangzhou, Guangdong 511447, China;2.National Quality Inspection and Testing Center for Processed Foods (Guangdong), Guangzhou, Guangdong 511447, China;3.Xiamen Medical College, Xiamen, Fujian 361023, China

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    摘要:

    目的 针对富硒食用油中硒形态检测的现有方法局限性,如硒形态相互转化、酶解时间长和可检测硒形态种类较少等问题,提出一种优化策略。方法 采用快速溶剂萃取法辅助蛋白酶K进行酶解,并建立高效液相色谱—电感耦合等离子体串联质谱法(HPLC-ICP-MS)。结果 40 ℃下,当蛋白酶K用量为35 mg、静态萃取时间为5 min时,硒形态提取率最高可达(83.65±2.36)%。8种硒形态目标物在20 min内可被有效分离,在2~100 μg/L范围内线性良好(R2≥0.999 3),检出限为0.20~0.60 μg/kg,定量限为0.60~1.80 μg/kg,加标回收率为82.3%~112.3%,相对标准偏差≤5.60%。结论 该方法提升了硒形态分析的效率和准确性。

    Abstract:

    Objective In this study, an optimized strategy was proposed to address the limitations of current methods for detecting selenium species in selenium-enriched edible oils, such as the transformation between selenium species, long enzymatic hydrolysis time, and the limited number of detectable selenium species.Methods Protease K-assisted hydrolysis was performed using accelerated solvent extraction, and a high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) method was established.Results At 40 ℃, with a proteinase K dosage of 35 mg and a static extraction time of 5 min, the extraction rate of selenium species could reach a maximum of (83.65±2.36)%. Eight target selenium species could be effectively separated within 20 min, with good linearity in the range of 2~100 μg/L (R2≥0.999 3), detection limits of 0.20~0.60 μg/kg, quantification limits of 0.60~1.80 μg/kg, spiked recovery rates between 82.3% and 112.3%, and relative standard deviations ≤5.60%.Conclusion This method improves the efficiency and accuracy of selenium speciation analysis.

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梁志森,张书迪,凌逍,等.快速溶剂萃取—高效液相色谱—电感耦合等离子体质谱法测定富硒食用油中8种硒形态[J].食品与机械,2025,(2):56-64.
LIANG Zhisen, ZHANG Shudi, LING Xiao, et al. Determination of eight selenium species in selenium-enriched edible oil with accelerated solvent extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometry[J]. Food & Machinery,2025,(2):56-64.

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  • 收稿日期:2024-12-03
  • 最后修改日期:2025-02-10
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  • 在线发布日期: 2025-04-03
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