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气相色谱-脉冲火焰光度法测定水产品中有机锡的研究

Study on Assay Method of Multicomponent Organotins in Aquatic Products by Gas Chromatography with Pulsed Flame Photometric Detector

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【作者】 赵孔祥赵云峰付武胜吴永宁

【Author】 ZHAO Kong-xiang,ZHAO Yun-feng,FU Wu-sheng,WU Yong-ning(National Institute for Nutrition and Food Safety,Chinese CDC,Beijing 100050,China)

【机构】 中国疾病预防控制中心营养与食品安全所福建省疾病预防控制中心中国疾病预防控制中心营养与食品安全所 北京100050天津出入境检验检疫局动植物与食品检测中心天津300457北京100050福建福州350003

【摘要】 目的建立气相色谱-脉冲火焰光度法(GC-PFPD)测定水产品中有机锡的研究。方法以氢溴酸+四氢呋喃(1+20)和0.03%环庚三烯酚酮-正己烷为萃取剂,凝胶渗透色谱法(GPC)净化,戊基溴化镁衍生后弗罗里硅土柱净化,气相色谱-脉冲火焰光度检测器(硫模式)检测。结果8种有机锡组分及内标分离良好,各组分相对响应因子的相对标准差(RSD)<15%,2种基质3个水平加标的平均回收率为84.1%~116.6%,RSD小于20%,标准参考物(ERM-CE477)中3种丁基锡测定结果与定值一致。结论气相色谱-脉冲火焰光度检器测定法满足了水产品中多组分有机锡痕量检测的需要。

【Abstract】 Objective To establish the method of multicomponent organotins in aquatic products by gas chromatography with pulsed flame photometric detector.Methods Hydrobromic acid+tetrahydrofuran(1+20)and 0.03% tropolone-hexane were used to extract three kinds of organotins from samples,and purified by gel-permeation chromatography in ethyl actate-tetrahydrofuran.The extracted compounds were derivatized by pentylmagnesium bromide.Organotins of extracted compound were separated by capillary column and detected by gas chromatography with pulsed flame photometric detector in sulfur mode.Results The RSDs of relative response factors of organotin compositions were less than 15%.The average recoveries of shellfish and fish for three spiked level were from 87.3% to 116.6% and RSDs were less than 20%.The detection results of 3 butyltins of standard reference material(ERM-CE477)were in agreement with the certified values.Conclusion The method could be applied to determination of organotins in aquatic products.

【基金】 科技部科学仪器设备升级改造专项“食品中有机锡超痕量检验用设备的改造(JG-2003-45)”;“十五”国家重大科技专项《食品安全关键技术》(2001BA804A19与2002BA804A45);福建省“沿海鱼贝类中有机锡化合物蓄积量及检验技术研究(2004Y015)”
  • 【文献出处】 中国食品卫生杂志 ,Chinese Journal of Food Hygiene , 编辑部邮箱 ,2008年02期
  • 【分类号】R155.5
  • 【被引频次】35
  • 【下载频次】305
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