色谱 ›› 2017, Vol. 35 ›› Issue (9): 907-911.DOI: 10.3724/SP.J.1123.2017.05013

• 研究快报 • 上一篇    下一篇

一种富集海水中有机氯和菊酯类农药的船载式正压固相萃取装置

叶江雷   

  1. 厦门海洋职业技术学院, 福建 厦门 361102
  • 收稿日期:2017-05-16 出版日期:2017-09-08 发布日期:2017-09-15
  • 通讯作者: 叶江雷,E-mail:yejianglei@126.com.
  • 基金资助:

    2015-福建省海洋与渔业结构调整专项资金(闽财指[2014]1084号);2015-度福建省海洋高新产业发展专项项目(闽海洋高新[2015]28号);厦门海洋学院2013~2014-度院级教科研项目(2013zk/yb-3).

A novel ship-borne positive pressure solid phase extraction device to enrich organo chlorinated and pyrethroid pesticides in seawater

YE Jianglei   

  1. Xiamen Ocean Vocational College, Xiamen 361102, China
  • Received:2017-05-16 Online:2017-09-08 Published:2017-09-15
  • Supported by:

    Special Fund for Ocean and Fishery Structure Adjustment in Fujian Province in 2015 (Fujian Financial Index No.[2014]1084); Special Project for Ocean High-Tech Industry Development of Fujian Province in 2015 (Fujian Ocean High-Tech No.[2015]28); 2013-2014 Annual College Level Teaching Research Project of Xiamen Ocean Vocational College (No. 2013zk/yb-3).

摘要:

研制了一种正压驱动的新型固相萃取(SPE)装置以替代真空泵负压驱动SPE装置用于富集海水中的有机氯和菊酯类农药。与水样接触的采样瓶和管路均采用不含氯的塑料材质。整个装置的连接部分用螺母螺栓紧固,以保证密封性和牢固性。水样瓶内部的压力(0.1~0.3 MPa)由单片机和压力传感器控制的隔膜充气泵(12 V电池供电)提供,水样过柱的流速在4.0~6.0 mL/min之间。SPE柱预淋洗后储存4周内有效,采样后储存6周内回收率大于80%。方法的线性关系良好,相关系数均大于0.9,方法的定量限为0.8~6.0 ng/L,3个不同添加水平(n=3)的平均回收率为86.1%~95.5%,相对标准偏差小于10%。海水实际样品中均检出六六六(BHC)和滴滴涕(DDT)。该装置在富集海水中有机氯和菊酯类农药方面有较好的应用。

关键词: 船载式, 富集, 海水, 菊酯类农药, 有机氯农药, 正压固相萃取

Abstract:

A novel solid phase extraction (SPE) device driven by positive pressure was developed instead of negative pressure from a vacuum pump, in order to enrich organo chlorinated and pyrethroid pesticides in seawater. The water sampling bottles and the pipelines which touch water samples were made of plastic material without chlorine. In order to ensure the sealing and firmness, the whole device were tightened with nut and bolt. The inner pressure (0.1-0.3 MPa) in the water sampling bottle was provided by the small air pump (powered by 12 V cell) controlled by a microprogrammed control unit (MCU) and pressure sensor to keep the water flow rate (4.0-6.0 mL/min). The pre-conditioned SPE column can be used for the enrichment of pesticides within four weeks, and the loaded SPE column can be eluted for detection within six weeks with recoveries greater than 80%. The linearity of the method was good with the correlation coefficient more than 0.9. The limits of quantification (LOQs) were 0.8-6 ng/L. The recoveries of the pesticides at three spiked levels (3 parallel samples) were 86.1%-95.5% with the relative standard deviations less than 10%. The benzene hexachlorides (BHCs) and dichloro-diphenyl-trichloroethanes (DDTs) were detected in seawater samples. The device has good application in enriching organo chlorinated and pyrethroid pesticides in seawater.

Key words: enrich, organo chlorinated pesticides, positive pressure solid phase extraction, pyrethroid pesticides, seawater, ship-borne

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