摘要
建立了气相色谱-质谱法同时测定食品中18种有机锡化合物含量的分析方法。样品以环庚三烯酚酮为络合剂,经甲醇-乙醇(80∶20,V/V)超声提取,通过四乙基硼化钠-四氢呋喃溶液衍生后用佛罗里硅土固相萃取柱净化,采用DB-5MS色谱柱分离,气相色谱-质谱联用仪测定,内标法定量。结果表明,18种有机锡在0.05~1.00 mg·L^(-1)线性关系良好,相关系数均在0.995以上。以青菜、苹果、稻谷、鱼肉和猪肉为代表性基质样品,在两个水平的添加浓度下,方法的回收率在81.61%~97.90%,相对标准偏差为0.19%~6.85%(n=6),18种有机锡的检出限均为0.02 mg·kg^(-1)。该方法可同时分析有机锡类农药残留和有机锡类环境污染物,分析效率更高,可更全面地评估食品中有机锡污染的风险。
An analytical method for the simultaneous determination of 18 organotin compounds in food by gas chromatography-mass spectrometry was established.The samples were extracted by ultrasonic extraction of methanol-ethanol(80∶20,V/V)with cycloheptactyltetraenolphenol as complexing agent,derivatized by tetraethylsodium boride-tetrahydrofuran solution,and purified by Florian silica solid-phase extraction column,separated by DB-5MS chromatography,measured by gas chromatography-mass spectrometry,and quantified by internal standard method.The results showed that the 18 organotins had a good linear relationship in the concentration range of 0.05 mg·L-1 to 1.00 mg·L-1,and the correlation coefficients were all above 0.995.The recoveries of the method ranged from 81.61%to 97.90%,the relative standard deviation ranged from 0.19%to 6.85%(n=6),and the detection limits of the 18 organotins were 0.02 mg·kg-1.This method can analyze organotin pesticide residues and organotin environmental pollutants at the same time,which is more efficient and can more comprehensively assess the risk of organotin contamination in food.
作者
胡婷婷
陈婷婷
许晓涵
熊珺
HU Tingting;CHEN Tingting;XU Xiaohan;XIONG Jun(Guangdong Dongguan Quality Supervision Testing Center,Dongguan 523808,China)
出处
《现代食品》
2025年第13期196-205,共10页
Modern Food
基金
东莞市社会发展科技项目(20211800905112)。
关键词
气相色谱-质谱法
食品
有机锡化合物
gas chromatography-mass spectrometry
food
organotin compounds