分散固相萃取-GC-MS法测定海产品中9种有机锡化合物  

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

作　　者：王姮 胡红美[2] 郭远明[2] 金衍健[2] 杨承虎[2] WANG Heng;HU Hong-mei;GUO Yuan-ming;JIN Yan-jian;YANG Cheng-hu(College of Food and Medicine,Zhejiang Ocean University,Zhoushan 316022,China;Marine Fisheries Research Institute of Zhejiang,Zhoushan 316021,China)

机构地区：[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

出　　处：《食品工业科技》2021年第1期233-238,共6页Science and Technology of Food Industry

基　　金：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)。

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10~1000μg/L,相关系数为0.9952~0.9988,检出限(3S/N)为0.4~1.0μg/kg dw(干重),以Sn计。在2.00、20.0和200μg/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~162.0μg/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。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 10~1000μg/L,the correlation coefficient was 0.9952~0.9988 and the detection limit(3S/N)was 0.4~1.0μg/kg(dry weight,calculated as Sn).The recoveries at the three added levels of 2.00,20.0,and 200μg/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~162.0μg/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.

关 键 词：海产品 有机锡化合物 分散固相萃取 超声波萃取 GC-MS 

分 类 号：TS[轻工技术与工程]