摘要
建立了QuEChERS净化结合超高效液相色谱-串联质谱(UHPLC-MS/MS)同时测定水产品中8种微囊藻毒素和2种腹泻性贝类毒素含量的方法。鲫鱼和白对虾样品采用95%甲醇提取,经无水MgSO_(4)、石墨化碳黑(GCB)及十八烷基硅烷键合硅胶(C_(18))吸附净化后,样液在0.1%甲酸水溶液(含5 mmol/L甲酸铵)-甲醇流动相体系下,经ACQUITY UPLC®HSS T3(2.1 mm×150 mm,1.8μm)色谱柱梯度洗脱分离。采用电喷雾正、负离子模式分别对10种藻毒素进行分析,多反应监测模式检测,外标法定量。结果表明,鲫鱼和白对虾基质中10种藻毒素在各自质量浓度范围内线性关系良好(r^(2)≥0.9990),检出限(LOD)和定量下限(LOQ)分别为0.1~5.0μg/kg和0.5~10μg/kg。3个不同加标水平下,鲫鱼、白对虾基质的平均回收率分别为79.5%~120%和73.2%~103%,相对标准偏差(RSD,n=6)分别为1.2%~14%和1.1%~16%。将该方法用于上海市售23份鲫鱼、2份花鲢和30份白对虾样品的分析,检出的藻毒素主要为MC-LR、MC-RR和MC-LF。该方法简单快速,灵敏度高,适用于水产品中10种藻毒素的定性鉴定和含量测定。
A reliable method was developed for the simultaneous determination of 8 microcystins and 2 diarrhoeal shellfish toxins in aquatic products by QuEChERS purification combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The Crucian carp and Litopenaeus vannamei samples were extracted with 95%methanol and purified by anhydrous Mg-SO_(4),graphitized carbon black(GCB)and octadecylsilane bonded silica gel(C_(18)).The filtrate was analyzed by a Waters ACQUITY UPLC®HSS T3 chromatographic column(2.1 mm×150 mm,1.8μm)with mobile phase consisting of 0.1%formic acid and 5 mmol/L ammonium formate and methanol.10 algal toxins were qualitatively and quantitatively analyzed by positive and negative electrospray ionization modes,detected by multiple reaction monitoring(MRM)mode and quantified by external standard method.The results showed that 10 algal toxins in Crucian carp and Litopenaeus vannamei showed good linear correlations with correlation coefficients(r^(2))not less than 0.9990 in the corresponding concentration ranges,and the limits of detection(LODs)and limits of quantitation(LOQs)were in the ranges of 0.1-5.0μg/kg and 0.5-10μg/kg,respectively.Average recoveries of the 10 algal toxins in Crucian carp and Litopenaeus vannamei at three different spiked levels were 79.5%-120%and 73.2%-103%,and the relative standard deviations(RSDs,n=6)were 1.2%-14%and 1.1%-16%,respectively.The established method was applied to the analysis of 23 samples of Crucian carp,2 Silver carp and 30 Litopenaeus vannamei samples in Shanghai,and MC-LR,MC-RR and MC-LF as the mainly detected algin toxins.This method is simple,rapid,effective,highly sensitive,and is suitable for the qualitative identification and content determination of 10 algal toxins in aquatic products.
作者
刘晓瑾
黄晴雯
郭大凯
王欣艺
陆思言
聂冬霞
韩铮
LIU Xiao-jin;HUANG Qing-wen;GUO Da-kai;WANG Xin-yi;LU Si-yan;NIE Dong-xia;HAN Zheng(School of Health Science and Engineering,University of Shanghai for Science and Technology,Shanghai 200093,China;Institute of Quality Standards and Testing Technology of Agricultural Products,Shanghai Academy of Agricultural Sciences,Shanghai 201403,China)
出处
《分析测试学报》
北大核心
2025年第10期2169-2176,共8页
Journal of Instrumental Analysis
基金
绿色食品(绿色优质农产品)高质量创新发展技术研究项目(GFJY2024007)
上海市农业科学院科研课题项目(农科应基2024(09))。
关键词
QUECHERS
超高效液相色谱-串联质谱法
微囊藻毒素
腹泻性贝类毒素
水产品
QuEChERS
ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)
microcystins(MCs)
diarrhetic shellfish poison(DSP)
aquatic products
