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

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％，兄如小于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。

Objective To establish the method of muhicomponent 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 actatetetrahydrofuran. 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 butyhins of standard reference material （ERM-CFA77） were in agreement with the certified values. Conclusion The method could be applied to determination of organotins in aquatic products.