【引用本文】 朱帅, 沈亚婷, 贾静, 等. 液相色谱-高分辨质谱法在中国东北地区农作物有机硒形态分析中的应用[J]. 岩矿测试, 2021, 40(2): 262-272. doi: 10.15898/j.cnki.11-2131/td.202005130070
ZHU Shuai , SHEN Ya-ting , JIA Jing , et al. Application of Liquid Chromatography-High Resolution Mass Spectrometry in Speciation Analysis of Organic Selenium in Crops in Northeast China[J]. Rock and Mineral Analysis, 2021, 40(2): 262-272. doi: 10.15898/j.cnki.11-2131/td.202005130070

液相色谱-高分辨质谱法在中国东北地区农作物有机硒形态分析中的应用

1. 自然资源部生态地球化学重点实验室, 国家地质实验测试中心, 北京 100037;

2. 桂林理工大学地球科学学院, 广西 桂林 541004

收稿日期: 2020-05-13  修回日期: 2020-09-29 

基金项目: 国家自然科学基金项目(21607033);中国地质调查局中国地质科学院基本科研业务费项目(CSJ201905)

作者简介: 朱帅,硕士,助理研究员,主要从事有机污染物与环境行为研究。E-mail:zhu15131215153@126.com。

Application of Liquid Chromatography-High Resolution Mass Spectrometry in Speciation Analysis of Organic Selenium in Crops in Northeast China

1. Key Laboratory of Eco-Geochemistry, Ministry of Natural Resources, National Research Center for Geoanalysis, Beijing 100037, China;

2. College of Earth Science, Guilin University of Technology, Guilin 541004, China

Received Date: 2020-05-13
Revised Date: 2020-09-29

摘要:随着公众对富硒产品的关注,对富硒农作物中硒含量的研究越来越受到人们的重视。针对现有方法测定农作物有机硒的基体效应和多原子离子质谱干扰问题,本研究利用液相色谱与抗干扰能力强的四极杆/静电场轨道阱高分辨质谱相结合,建立了农产品中有机硒的形态分析方法。经优化以超声波辅助蛋白酶XIV提取农作物中有机硒,用Waters Symmetry RP18液相色谱柱分离,以纯水和乙腈作为流动相进行梯度洗脱,采用正、负离子切换同时测定了硒代蛋氨酸、硒代胱氨酸、甲基硒代半胱氨酸。3种有机硒在负离子模式下采用Full MS/dd-MS2扫描模式对目标物进行定性筛查和确证,3种有机硒在5~500μg/L的浓度范围内线性关系良好,相关系数均大于0.997,检出限为1.0~4.7μg/kg,回收率为76.4%~116.0%,相对标准偏差 ≤ 6.5%。与现有方法比较,本方法线性范围宽,适用于多种谷物和蔬菜类样品的分析。将建立的方法应用于测定中国粮食主产区东北黑龙江地区多种农作物的可食部分,结果发现谷类中以硒代蛋氨酸为主,蔬菜类以甲基硒代半胱氨酸为主,并且该地区农作物的有机硒含量处于较低水平,亟待强化补硒。

关键词: 有机硒, 农作物, 四极杆/静电场轨道阱高分辨质谱法, 超声酶提取

Application of Liquid Chromatography-High Resolution Mass Spectrometry in Speciation Analysis of Organic Selenium in Crops in Northeast China

KEY WORDS: organic selenium, crop, quadrupole/obitrap high-resolution mass spectrometry, ultrasonic enzyme extraction

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液相色谱-高分辨质谱法在中国东北地区农作物有机硒形态分析中的应用

朱帅, 沈亚婷, 贾静, 劳昌玲