气相色谱分析中样品前处理装置的研制  

Development of Sample Preprocessing Method for Gas Chromatography

作　　者：杨志岩[1] 闫仲丽[1] 王建清[1] 

机构地区：[1]天津科技大学,天津300457

出　　处：《现代科学仪器》2008年第4期67-69,共3页Modern Scientific Instruments

基　　金："十五"国家科技攻关重大项目:科学仪器研制与开发<样品自动化前处理设备的研制与开发>;(2004BA210A05)。

摘　　要：探索一种新型的样品前处理装置,首次运用载体、携带体和综合蒸馏技术完成了待测样品中微量成分的提取分离和富集。将冷端接受器设计为可更换结构,所以无样品交叉干扰,适用于痕量组分的富集。在乙酸乙酯中添加了4种微量有机磷农药后进行了前处理,其装置能自动将微量组分富集到2 mL邻苯二甲酸二甲酯中。利用气相色谱分析的结果,研究了样品前处理装置分离富集参数的选择原则。实验证实,该方法能最有效地除去蛋白、脂肪、色素等对气相色谱分析有干扰的组分;将待测微量组分的浓度富集150倍以上;回收率90-117%;相对标准偏差1.3-10%;最小检出浓度1 ng/mL。有机试剂的回收利用率大于95%,而且操作简单方便,以模拟试样为例说明了方法的实用性。This paper investigates a new Sample Preprocessing device. Support, delivery and compositive distillation technique was first used to complete the extraction, separation and concentration of trace components. Cold junction of the device was exchangeable, so there was no cross interference, and it was fit for concentration of trace components. After adding four kinds of minor organophosphorus pesticides, acetic ester was preprocessed. The distillate was analyzed by gas chromatography and the principle of choosing parameters for the device was studied. It was proven that the interferential components to gas chromatography such as protein, lipid and pigment could be removed effectively, trace target components could be concentrated more than 150 folds, recoveries were from 90% to 117% , and the relative standard deviation （RSD） was from 1.3% to 10%, the limit of determination （LOD） of this method was 1ng/mL, reused rate of organic reagent was more than 95%. Practicability of the method was illustrated with the examole of analog samole.

关 键 词：气相色谱 载体 携带体 综合蒸馏 样品前处理 富集 

分 类 号：O657.71[理学—分析化学]