分散固相萃取-GC-MS法测定海产品中9种有机锡化合物

王姮; 胡红美; 郭远明; 金衍健; 杨承虎

doi:10.13386/j.issn1002-0306.2020030184

分散固相萃取-GC-MS法测定海产品中9种有机锡化合物

doi: 10.13386/j.issn1002-0306.2020030184

1. 浙江海洋大学食品与医药学院, 浙江舟山 316022;
2. 浙江省海洋水产研究所, 浙江舟山 316021

基金项目:

国家自然科学基金（31800430）；浙江省科协育才项目（2017YCGC013）；舟山市科技项目（2016C31055）；舟山市科技计划项目（2019C31048）。

详细信息

作者简介:
王姮(1994-),女,硕士研究生,研究方向:水产品质量与安全评价,E-mail:wangh2607@163.com。

通讯作者:
胡红美(1986-),女,博士研究生,高级工程师,研究方向:海洋环境及食品安全分析,E-mail:huhm@zju.edu.cn。

中图分类号: TS
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出版历程
- 收稿日期: 2020-03-16

Detection of Nine Organotin Compounds in Seafood by Dispersive Solid Phase Extraction Combined with Gas Chromatography Mass Spectrometry

1. College of Food and Medicine, Zhejiang Ocean University, Zhoushan 316022, China;
2. Marine Fisheries Research Institute of Zhejiang, Zhoushan 316021, China

摘要

摘要: 本实验建立了一种同时检测海产品中9种有机锡化合物的新方法。样品依次经过超声波提取，冷冻脱脂，N-丙基乙二胺（PSA）分散固相萃取、四乙基硼酸钠衍生、石墨化炭黑（GCB）分散固相萃取，最后采用气相色谱-质谱法（GC-MS）进行测定。在优化条件下，9种有机锡化合物的线性范围为10~1000 μg/L，相关系数为0.9952~0.9988，检出限（3S/N）为0.4~1.0 μg/kg dw （干重），以Sn计。在2.00、20.0和200 μg/kg 3个添加水平的回收率为81.2%~115.0%，相对标准偏差为4.1%~7.5%（n=5）。对龙头鱼、梅童鱼、小黄鱼、大黄鱼、带鱼、鲳鱼、海鳗、哈氏仿对虾、口虾蛄、梭子蟹、缢蛏、牡蛎等海产品中9种有机锡化合物进行检测，结果表明梅童鱼、小黄鱼、大黄鱼、海鳗中均未检出9种有机锡化合物。在龙头鱼、带鱼、鲳鱼、哈氏仿对虾、口虾蛄、梭子蟹、缢蛏、牡蛎中9种有机锡化合物总量为ND~162.0 μg/kg ww （湿重），以Sn计。该方法简捷高效，基体干扰小，可用于海产品样品中的9种有机锡化合物的同时检测。
- 海产品 /
- 有机锡化合物 /
- 分散固相萃取 /
- 超声波萃取 /
- GC-MS
Abstract: A method was developed for the simultaneous detection of nine organotin compounds in seafood. The samples were subjected to ultrasonic extraction,freeze degreasing,N-propylethylenediamine(PSA)dispersive solid phase extraction,sodium tetraethylborate derivative,graphitized carbon black(GCB)dispersive solid phase extraction,and finally analyzed by gas chromatography-mass spectrometry(GC-MS). Under the optimized conditions,the linear range of the nine organotin compounds was 10~1000 μg/L,the correlation coefficient was 0.9952~0.9988 and the detection limit(3S/N)was 0.4~1.0 μg/kg(dry weight,calculated as Sn). The recoveries at the three added levels of 2.00,20.0,and 200 μg/kg were 81.2%~115.0%,and the relative standard deviations were 4.1%~7.5%(n=5). Nine kinds of organotin compounds were tested in seafood such as Bombay duck,Collichthys niveatus,small yellow croaker,big yellow croaker,largehead hairtail,pomfret,moray eel,Parapenaeopsis hardwickii,mantis shrimp,port crab,Sinonovacula constricta and oyster,the results showed that nine kinds of organotin compounds were not detected in Collichthys niveatus,small yellow croaker,big yellow croaker and moray eel. The total amount of nine kinds of organotin compounds in Bombay duck,largehead hairtail,pomfret,Parapenaeopsis hardwickii,mantis shrimp,port crab,Sinonovacula constricta and oyster was ND~162.0 μg/kg(wet weight,as Sn). This method is simple and efficient,and has low matrix interference. It can be used for the simultaneous detection of nine organotin compounds in seafood samples.
- seafood /
- organotin compounds /
- dispersive solid phase extraction /
- ultrasonic extraction /
- GC-MS

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