Xu Xiaoqin, Yang Huanghao, Wang Ling, Han Bin, Wang Xiaoru, Lee Frank Sen-Chun
Department of Chemistry and the Key Laboratory of Analytical Science of the Ministry of Education, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China.
Anal Chim Acta. 2007 May 15;591(1):87-96. doi: 10.1016/j.aca.2007.03.044. Epub 2007 Mar 25.
A solid-phase microextraction (SPME) method has been developed for the determination of 3 chloroacetanilide herbicides in both fresh and seawater samples. The extracted sample was analyzed by gas chromatography with mass spectrometry detection (GC-MS), and parameters affecting SPME operation including fibre type, sample pH, sample temperature, mixing speed and extraction time have been evaluated and optimized. The amount of dissolved organic matter (DOM) and the salt content both affected SPME extraction efficiency, but the presence of other competitive extractants such as organochlorine pesticides (OCPs) in the matrix showed no insignificance interference. The limit of detection (LOD) for acetochlor, metolachlor and butachlor were 1.2, 1.6 and 2.7 ng L(-1), respectively. The recoveries for the herbicides ranged from 79 to 102%, and the linear dynamic range was from 10 to 1000 ng L(-1). The developed method has been used to monitor herbicides contaminations in coastal water samples collected around Laizhou bay and Jiaozhou bay in Shandong peninsula, China. The concentrations of acetochlor and metolachlor ranged from undetectable to 78.5 ng L(-1) and undetectable to 35.6 ng L(-1), respectively. Butachlor was not observed but in only one sample and the concentration is lower than the limit of quantification (LOQ). The concentrations of the three herbicides in this study are low compared to most of the other places reported.
已开发出一种固相微萃取(SPME)方法,用于测定淡水和海水样品中的3种氯代乙酰苯胺类除草剂。萃取后的样品通过气相色谱-质谱检测(GC-MS)进行分析,并对影响SPME操作的参数(包括纤维类型、样品pH值、样品温度、混合速度和萃取时间)进行了评估和优化。溶解有机物(DOM)的量和盐含量均影响SPME的萃取效率,但基质中其他竞争性萃取剂(如有机氯农药(OCPs))的存在未显示出显著干扰。乙草胺、异丙甲草胺和丁草胺的检测限(LOD)分别为1.2、1.6和2.7 ng L⁻¹。除草剂的回收率在79%至102%之间,线性动态范围为10至1000 ng L⁻¹。所开发的方法已用于监测中国山东半岛莱州湾和胶州湾周边采集的沿海水样中的除草剂污染情况。乙草胺和异丙甲草胺的浓度分别在未检出至78.5 ng L⁻¹和未检出至35.6 ng L⁻¹之间。仅在一个样品中检测到丁草胺,其浓度低于定量限(LOQ)。与其他大多数报道的地方相比,本研究中这三种除草剂的浓度较低。