摘要
基于液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS),比较了两种亲水交互作用(hydrophilic liquid interaction chromatography column,HILIC)色谱柱和C18色谱柱分析扁玉螺(Neverita didyma)、脉红螺(Rapana venosa)、栉江珧(Atrina pectinata)和菲律宾蛤仔(Ruditapes philippinarum)等贝类样品中神经毒素β-N-甲氨基-L-丙氨酸(β-N-methylamino-L-alanine,BMAA)及其同分异构体化合物的性能。本研究采用Agilent 6430串联质谱对3批扁玉螺样品中的游离态、总溶解态和沉淀结合态BMAA毒素进行了分析,通过AB Sciex Qtrap 4500质谱分析了其他3种贝类样品的总溶解态BMAA。结果表明,4种贝类样品均含有BMAA和低浓度的2,4-二氨基丁酸(2,4-diaminobutyric acid,DAB),且扁玉螺中的β-氨基-N-甲基丙氨酸(β-amino-N-methylalanine,BAMA)含量较低,其他3种贝类含有较高浓度的BAMA,但均未检出N-2-氨乙基甘氨酸[N-(2-aminoethyl)glycine,AEG]。HILIC-MS/MS直接分析法获得的定量结果均高于AQC-柱前衍生法的定量结果,建议使用HILIC-MS/MS直接分析法对生物样品中的BMAA进行定性和定量分析,采用变迁离子119->88和119->44的信号强度辅助定性,并使用前者的色谱峰面积进行定量计算,条件允许时可采用AQC-柱前衍生法进行辅助定性分析。本研究可为生物样品中BMAA毒素的检测分析提供重要的方法学参考。
Based on the liquid chromatography-tandem mass spectrometry(LC-MS/MS)system,two hydrophilic liquid interaction chromatography(HILIC)columns and a C18 column were respectively used and compared the analytical performance for the analysis of the neurotoxinβ-N-methylamino-L-alanine(BMAA)and its isomers in mollusk samples(Neverita didyma,Rapana venosa,Atrina pectinata,and Ruditapes philippinarum).The analytical methods developed on an Agilent 6430 tandem mass spectrometer were used to analyze the free form,total soluble form,and precipitate-bound form of BMAA in three batches of N.didyma,and the other methods developed on an AB Sciex Qtrap 4500 tandem mass spectrometer were adopted to analyze the total soluble form of BMAA in three species of mollusks including R.venosa,A.pectinata,and R.philippinarum.The results indicated that BMAA and trace amounts of 2,4-diaminobutyric acid(DAB)were shown in all mollusk samples,and another isomer of BMAA,β-amino-N-methylalanine(BAMA),was present in N.didyma with low content but more content of BAMA was detected in the other mollusk samples.However,N-(2-aminoethyl)glycine(AEG),an isomer of BMAA,was not detected in all tested samples.The quantitative results of BMAA obtained by the HILIC-MS/MS direct analysis method were totally higher than that acquired by the precolumn AQC-derivatization method.This study suggested that the HILIC-MS/MS direct analysis method developed on the AB Sciex mass spectrometer could be used to analyze BMAA in biological samples,the intensity ratios between the transition ions 119->88 and 119->44 could be used to assist qualitative analysis of BMAA,and the former transition ions could be adopted to quantify the target compound.The precolumn AQC-derivatization method could be used for qualitative analysis of BMAA,which provided an important methodological reference for the determination and analysis of BMAA toxin in biological samples.
作者
王超
邱江兵
宋甲亮
李爱峰
WANG Chao;QIU Jiangbing;SONG Jialiang;LI Aifeng(College of Environmental Science and Engineering, Ocean University of China, Qingdao 266100, China;Key Laboratory of Marine Environment and Ecology, Ocean University of China, Ministry of Education, Qingdao 266100, China)
出处
《中国渔业质量与标准》
2021年第1期34-45,共12页
Chinese Fishery Quality and Standards
基金
国家自然科学基金面上项目(41676093)
中央高校基本科研业务费专项(201841003)。
