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超声波提取-气相色谱-质谱法测定紫菜中甲基锡及乙基锡
Simultaneous determination of three organotin compounds in laver by gas chromatography-mass spectrometry
【摘要】 建立了紫菜中二甲基锡、三甲基锡和三乙基锡的同时检测新方法。紫菜样品经过超声波辅助提取,采用四乙基硼酸钠对紫菜样品提取液中的有机锡化合物进行衍生后,经活性炭净化,运用气相色谱-质谱法(GC-MS)进行分析。在优化条件下,3种有机锡化合物在0.02~2.5 mg·L-1的范围内得获得了较好的线性,检测限分别为0.004 3、0.003 8和0.002 6mg·L-1,其相关系数分别为0.998 0、0.999 1和0.998 5。二甲基锡、三甲基锡和三乙基锡在0.05、0.50和2.0 mg·L-1 3个添加水平的平均回收率为72.6%-95.7%,相对标准偏差为5.14%-9.26%。该方法可以用于紫菜样品中多种有机锡化合物的同时检测。
【Abstract】 The protocol for simultaneous determination and quantification of 3organotins in laver samples was established by using gas chromatography-mass spectrometry(GC-MS)techniques.The laver samples were extracted by ultrasonic assisted extraction,and derivatized with sodium tetraethylborate(NaBEt4).The extracts were analyzed by GC-MS after being purified with graphitized carbon black.Under the optimized conditions,good accuracy and specificity were achieved.The average recovery rate obtained for the analytes was in the range of 72.6%-95.7%,with the relative standard deviations(RSDs)lower than 9.26%.The limits of detection for each OTC were 0.0043,0.003 8mg·L-1 and 0.0026mg·L-1,respectively.Some different laver samples were also detected using this developed method.It is expected that this method could be used for the OTCs determination in the future.
【Key words】 Dimethyltin; Trimethyltin; Triethyltin; Gas chromatography-Mass spectrometry; Laver;
- 【文献出处】 南昌大学学报(理科版) ,Journal of Nanchang University(Natural Science) , 编辑部邮箱 ,2014年06期
- 【分类号】TS255.7;O657.63
- 【被引频次】5
- 【下载频次】48