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基于电子鼻和HS-SPME-GC-MS方法研究 海水中七氯的快速检测技术
何红萍1, 周 君1, 李 晔1, 张春丹1, 黄 健2, 缪芳芳1, 苏秀榕1, 李太武3
1.宁波大学海洋学院;2.北京普析通用仪器有限责任公司;3.宁波城市职业技术学院
摘要:
为了建立海水中有机氯农药的快速检测技术, 本文基于电子鼻和顶空固相微萃取气质联用法(HS-SPME-GC-MS)对海水中的七氯进行检测。结果表明, 电子鼻可以识别海水中的挥发性七氯成分及浓度, 最低检测限0.01mg/L。利用线性判别分析方法(LDA)的累计判别贡献率和欧氏距离、判别函数法、相关性对未知样品的识别率均达到了80%以上, 具有良好的区分效果; PLS模型预测七氯浓度跟实际值之间的相对误差在0.49%—16%之间。HS-SPME-GC-MS检测浓度小于0.10mg/L时, 相对误差在10%左右; 而大于此浓度时, 相对误差随之增大。检测到的主要挥发性物质基本呈现规律性的变化, 与电子鼻确认结果一致。对比两种检测技术, 发现电子鼻检测方法比HS-SPME-GC-MS更迅速、灵敏, 检测限更低, 相对误差也更小, 仪器便携、投资相对较小。
关键词:  七氯  顶空固相微萃取-气质联用  电子鼻  定性和定量
DOI:10.11693/hyhz201305033033
分类号:
基金项目:海洋公益性行业科研专项经费资助项目, 201005016号; 宁波大学学科项目, 2010597号。
THE METHOD RESEARCH OF HEPTACHLOR IN SEAWATER BY COMBINATION OF ELECTRONIC NOSE AND HS-SPME-GC-MS
HE Hong-Ping1, ZHOU Jun1, LI Ye1, ZHANG Chun-Dan1, HUANG Jian2, MIAO Fang-Fang1, SU Xiu-Rong1, LI Tai-Wu3
1.School of Marine Sciences, Ningbo University;2.Beijing Purkinje General Instrument Co., Ltd.;3.Ningbo College of Vocational Technology
Abstract:
To establish rapid detection technology of Organochlorine pesticides in seawater in this paper, based on Electric nose and headspace-solid phase micro-extraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS), detect the different concentrations in seawater. The results showed that electric nose can be used to distinguish the volatile components and concentration of Heptachlor in different seawater, and the lowest detectable limit reached 0.01mg/L. The accumulative contribution rate of discrimination of LDA and the recognition rate were both achieved to over 80% among the test methods like Euclidean distance, discriminant function method and correlations, the analysis detected well. In PLS model, the relative error between Heptachlor concentration of the prediction and the actual value was between 0.49% to 16%. The relative error was less than 10% in the HS-SPME-GC-MS detection, less than 0.1mg/L concentration level; the relative error increased when the sample was more than 0.1mg/L levels. The main volatile substances detected showed predictable changes, consistent with the confirmation results by electronic nose. Comparing the two kinds of detection technology, results show that the electronic nose detection is more rapid, sensitive, lower detection limit and the relative error is smaller. Besides that, the instrument is portable and relatively less expensive.
Key words:  Heptachlor  HS-SPME-GC-MS  Electronic nose  qualitative and quantitative
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