高效液相色谱串联质谱法检测富硒药食用蕈菌产品中有机硒含量  

Determination of Organic Selenium Content in Selenium Rich Medicines and Edible Mushroom Products by High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：严美婷 刘春兰 邓珊 毛自欣 李崇香 李琎杰 YAN Meiting;LIU Chunlan;DENG Shan;MAO Zixin;LI Chongxiang;LI Jinjie(Food Inspection and Testing Institute of Jiangxi General Institute for Inspection,Testing and Certification,Yichun 336000,China;School of Chemistry and Bioengineering,Yichun University,Yichun 336000,China)

机构地区：[1]江西省检验检测认证总院食品检验检测研究院,江西宜春336000 [2]宜春学院化学与生物工程学院,江西宜春336000

出　　处：《食品科技》2024年第4期32-36,共5页Food Science and Technology

基　　金：江西省药品监督管理局科研项目(2023JS29);江西省科技计划项目(20192bBBFL60033);江西省富硒食品质量检验检测中心(宜春)项目。

摘　　要：文章建立了一种灵敏度高、简洁快速测定富硒药食用蕈菌产品中硒形态及其含量的高效液相色谱串联质谱分析方法。通过对比水提取法、酸提取法和酶解提取法3种前处理方法对蛹虫草硒多肽片样品中硒代氨基酸的提取效果,并选取Agilent ZORBAX SB-AQ亲水色谱柱(柱长100 mm,内径3.0 mm,粒径1.8μm),1%甲酸水和甲醇流动相梯度洗脱,在柱温35℃、流量0.2 mL/min条件下检测样品中的3种硒代氨基酸。结果表明,3种提取方法中,酶解提取法提取效率最高,能较好地提取蛹虫草硒多肽片中硒代氨基酸,采用高效液相色谱串联质谱法检测3种氨基酸在0.5~100 ng/mL浓度范围呈现较好的线性关系,平均回收率分别为93.9%、94.2%、93.8%,相对标准偏差分别为3.42%、2.95%、2.13%。该方法简单、快速、准确,可实现大批量多样品的检测,为我国富硒产品质量安全监管方面提供技术参考。A high performance liquid chromatography tandem mass spectrometry(HPLC-MS)analysis method has been established for the determination of selenium forms and content in selenium rich medicinal and edible mushroom products.This method has the advantages of high sensitivity,simplicity and speed.By compared the extraction effects of seleno-amino acids from the selenium peptide tablet samples of Cordyceps militaris using three different pre-treatment methods:water extraction,acid extraction,and enzymatic hydrolysis extraction,and selected an Agilent ZORBAX SB-AQ hydrophilic chromatographic column(100 mm in length,3.0 mm in diameter and 1.8μm in particle size),used 1%formic acid water and methanol mobile phase gradient elution,three seleno-amino acids were detected in the sample under column temperature of 35℃and flow rate of 0.2 mL/min.The results showed that among the three extraction methods,the enzymatic extraction method had the highest extraction efficiency and could effectively extract seleno-amino acids from the selenium peptide tablets of Cordyceps militaris.The detection of three amino acids using HPLC-MS showed a good linear relationship in the concentration range of 0.5–100 ng/mL,and the average recovery rates were 93.9%,94.2%,93.8%,the relative standard deviations were 3.42%,2.95%and 2.13%.This method is simple,fast,and accurate,and can achieve the detection of multiple samples,provide technical reference for the quality and safety supervision of selenium rich products in China.

关 键 词：高效液相色谱串联质谱法 富硒药食用蕈菌 有机硒 酶解提取法 

分 类 号：TS207.3[轻工技术与工程—食品科学]