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  

Determination of eight selenium species in selenium-enriched edible oil with accelerated solvent extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometry

作　　者：梁志森 张书迪 凌逍 陈玉珍 LIANG Zhisen;ZHANG Shudi;LING Xiao;CHEN Yuzhen(Guangzhou Inspection and Testing Certification Group Company Limited,Guangzhou,Guangdong 511447,China;National Quality Inspection and Testing Center for Processed Foods(Guangdong),Guangzhou,Guangdong 511447,China;Xiamen Medical College,Xiamen,Fujian 361023,China)

机构地区：[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

出　　处：《食品与机械》2025年第2期56-64,共9页Food and Machinery

基　　金：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)。

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2~100μg/L范围内线性良好(R^(2)≥0.9993),检出限为0.20~0.60μg/kg,定量限为0.60~1.80μg/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。[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 2~100μg/L(R^(2)≥0.9993),detection limits of 0.20~0.60μg/kg,quantification limits of 0.60~1.80μg/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.

关 键 词：硒形态 电感耦合等离子体质谱法 混合模式色谱 动态反应池 有机进样 快速溶剂 

分 类 号：O65[理学—分析化学]