摘要
建立了紫菜中三丁基锡(TBT)和三苯基锡(TPhT)化合物同时分析的气相色谱法。样品以乙酸乙酯-正己烷(体积比为4∶1)超声提取,四乙基硼酸钠衍生,衍生物经活性炭固相材料分散净化后,用响应面分析法对提取条件进行优化,最后采用气相色谱-火焰光度法(GC-FPD)测定。研究结果表明,TBT、TPhT这两种有机锡化合物在0.1～10mg/L浓度范围内均线性良好,其相关系数分别为0.9989和0.9996;检测限分别为0.038和0.049mg/L。在三个不同添加水平下,TBT、TPhT的平均回收率范围为80.3%～106.9%,相对标准偏差为5.1%～8.7%。该方法快速、准确,可应用于紫菜中TBT、TPhT的同时检测。
A method for simultaneous determination of tributyltin（TBT） and triphenyltin （TPhT） in laver by GC-FPD was developed. The sample was ultrasonically extracted with ethyl acetate-hexane （4/1 ,V/V） and derivatized with NaBEt4 ,followed by the dispersive solid phase extraction clean-up using activated carbon as solid phase material. The sample extracts were finally determined by GC-FPD and the response surface analysis was used to optimize the extraction conditions of TBT and TPhT. The method showed good linearities between analytical signals and analyte concentrations in the range of 0. 1-10 mg/L with the correlation coefficients of 0. 9989-0. 9996. For TBT and TPhT, the detection limits were 0. 038 and 0. 049 mg/L, respectively. In three spiked levels, the average recoveries of tributyltin and triphenyltin ranged from 80.3%-106.9% with relative standard derivation（RSD） of 5.1%-8.7%. The proposed method was successfully applied to the determination of TBT and TPhT in real samples. The results indicate this method is rapid,accurate and can be used to detect TBT and TPhT in laver.
出处
《分析科学学报》
CAS
CSCD
北大核心
2012年第6期757-761,共5页
Journal of Analytical Science
基金
国家自然科学基金(No.20965005)
江西省科技支撑计划(No.2008BB22400)
南昌大学食品科学与技术国家重点实验室目标导向项目(No.SKLF-MB-201002)
南昌大学食品科学与技术国家重点实验室自由探索项目(No.SKLF-TS-200918)
关键词
三丁基锡
三苯基锡
超声波提取
分散固相萃取
气相色谱法
响应面分析
Tributyltin
Triphenyltin
Ultrasound-assisted extraction
Dispersive solid phase extraction
Gas chromatography
Response surface analysis
