摘要
目的建立同时测定贝类食品中10种脂溶性贝类毒素(LSTs)的高效液相色谱-串联质谱方法。方法样品中脂溶性贝类毒素采用甲醇提取、氢氧化钠溶液皂化后,通过固相萃取净化,经BEH C18色谱柱(50 mm×2.1 mm,1.7μm)分离,电喷雾正/负离子多反应监测(MRM)模式检测,基质匹配曲线外标法定量。结果 10种毒素的线性方程相关系数均在0.999以上,定量限为0.7μg/kg~3.0μg/kg,线性范围为1.0μg/kg~96μg/L。贻贝、牡蛎、扇贝3种贝类的平均加标回收率分别为90.6%~123%、79.2%~126%、88.2%~125%,相对标准偏差为1.08%~11.8%。将方法应用于100份贝类样品的检测,其中有60份检测出homo虾夷扇贝毒素(h YTX),最高含量为533.4μg/kg,另各有1份贻贝样品分别检测出YTX和罗环内脂毒素(SPX1),含量分别为8.9μg/kg和2.8μg/kg。结论本方法高效灵敏、快速简便,适用于双壳贝类中的脂溶性贝类毒素的日常检测分析。
Objective A method was developed for the simultaneous determination of 10 lipophilic shellfish toxins by using liquid chromatography-tandem mass spectrometry( LC-MS/MS). Methods To extract the LSTs,shellfish were treated with methanol and saponified further with sodium hydroxide solution,the extraction were then purified by SPE. After all these pretreatment processes,all the determine and were separated on a BEH C18 column( 50 mm × 2. 1 mm,1. 7 μm),and detected by electrospray ionization positive/negative multiple reaction monitoring( MRM) mode,then quantitated by matrix matching curve external standard method. Results The correlation coefficients of the linear equation of the 10 toxins are all above0. 999,the limits of quantifications are within 0. 7 μg/kg-3. 0 μg/kg,and the linear ranges are within 1. 0 μg/L-96 μg/L.The average recovery rate of mussel,oyster and scallop were within 90. 6%-123%,79. 2%-126%,88. 2%-125%,respectively and the relative standard deviation was within 1. 08%-11. 8%. The method was applied to the detection of 100 shellfish samples,60 of which showed the positive expression of detected h YTX and the highest content was 533. 4 μg/kg. In addition,YTX and SPX1 were respectively detected in one mussel sample,with contents of 8. 9 μg/kg and 2. 8 μg/kg.Conclusion This method is efficient,sensitive,fast and simple,and is suitable for the daily monitoring and analysis of lipophilic shellfish toxins in bivalve shellfish.
作者
何明珠
秦逍云
刘桂华
杨胜园
刘红河
袁冠湘
HE Ming-zhu;QIN Xiao-yun;LIU Gui-hua;YANG Sheng-yuan;LIU Hong-he;YUAN Guan-xiang(College of Public Health,University of South China,Hengyang,Hunan 421001,China;不详)
出处
《中国卫生检验杂志》
CAS
2021年第4期397-402,406,共7页
Chinese Journal of Health Laboratory Technology
基金
国际原子能机构合作研究基金IAEA Research Contract No:18859。
关键词
脂溶性贝类毒素
液相色谱-串联质谱法
贝类
Lipophilic shellfish toxins
Liquid chromatography-tandem mass spectrometry
Shellfish
