气相色谱法测定洞头海域海水中16种有机氯农药残留量  

Determination of 16 organochlorine pesticide residues in seawater of Dongtou sea area by gas chromatography

作　　者：李妃 陶建斌 柯志恒 杨丽君 LI Fei;TAO Jian-bin;KE Zhi-heng;YANG Li-jun(Dongtou District Center for Disease Control and Prevention,Wenzhou,Zhejiang 325400,China;不详)

机构地区：[1]温州市洞头区疾病预防控制中心,浙江温州325400 [2]温州市洞头区霓屿街道办事处,浙江温州325400

出　　处：《中国卫生检验杂志》2021年第17期2060-2063,共4页Chinese Journal of Health Laboratory Technology

基　　金：温州市洞头区科技计划项目(S2017S29B)。

摘　　要：目的建立海水中16种有机氯农药的气相色谱-电子捕获检测器测定方法。方法海水样品经液-液萃取、固相萃取净化、氮吹浓缩等前处理后利用GC-ECD进行分析测定,色谱系统采用DB-1701毛细管色谱柱(30 m×0.32 mm,0.25μm);柱温为程序升温,初始温度100℃,以15℃/min升温至200℃,保持10 min,然后以10℃/min速率升至250℃,保持8 min;进样口温度260℃。结果在0.75μg/L~200μg/L浓度内,16种有机氯农药的线性关系良好,相关系数为0.999 1~0.999 9;方法检出限在0.53 ng/L~2.90 ng/L;在0.5μg/L、10μg/L、50μg/L 3个浓度水平的加标浓度下,平均回收率为82.0%~107.9%,相对标准偏差为2.46%~9.21%。为了解洞头养殖海域水体有机氯农药的污染现状,采用所建立的方法对采集的24份不同养殖区的海水样品进行检测,结果均未检出。结论该方法灵敏、简便、准确,适用于海水中有机氯农药的定性定量分析。Objective To establish a method to determinate 16 organochlorine pesticides(OCPs)residues in seawater by gas chromatography with electron-capture detection(GC-ECD).Methods The samples were firstly extracted by liquid-liquid extraction,then cleaned-up by solid phase extraction(SPE)and concentrated under nitrogen flow,finally determined with GC-ECD method.The DB-1701 gas chromatography column(30 m×0.32 mm,0.25μm)was used.The column temperature was programming increased with initial temperature of 100℃and raising to 200℃with a rate of 15℃/min,maintaining for 10 min,then raised to 250℃with a rate of 10℃/min to keep 8 min.The inlet temperature was 260℃.Results The linearity was good when the concentrations of 16 organochlorine pesticides were within 0.75μg/L-200μg/L,and the correlation coefficient was within 0.9991-0.9999.The detection limit of the method was within 0.53 ng/L-2.90 ng/L.The average recoveries ranged from 82.0%to 107.9%at the spiked concentration of 0.5μg/L,10μg/L and 50μg/L,and the relative standard deviations ranged from 2.46%to 9.21%.In order to understand the pollution status of organochlorine pesticides in the waters of Dongtou sea area,24 samples of seawater collected from different aquaculture areas were tested by the established method,and the results were not detected.Conclusion This method is simple,sensitive and accurate,which is suitable for the determination of OCPs in seawater.

关 键 词：海水 有机氯农药 气相色谱法 

分 类 号：O657.71[理学—分析化学]