广西师范大学学报（自然科学版） ›› 2017, Vol. 35 ›› Issue (2): 93-100.doi: 10.16088/j.issn.1001-6600.2017.02.014

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扫集-胶束电泳检测鱼塘水中季铵盐类除草剂

张庆庆1, 王燕燕2, 孟品佳1*, 张文芳2   

  1. 1.中国人民公安大学刑事技术学院,北京100038;
    2.北京市公安局司法鉴定中心,北京100192
  • 出版日期:2017-07-25 发布日期:2018-07-25
  • 通讯作者: 孟品佳(1955—),女,辽宁沈阳人,中国人民公安大学教授。E-mail:mengpinjia@163.com
  • 基金资助:
    国家重大科学仪器设备开发专项(2013YQ090875-12)

Determination of Quaternary Ammonium Herbicides in Pond Water by SPEwith Sweeping-MEKC Method

ZHANG Qingqing1,WANG Yanyan2,MENG Pinjia1*, ZHANG Wenfang2   

  1. 1.Department of Forensic Science,Chinese People’s Public Security University,Beijing 100038, China;
    2. Forensic Science Service of Beijing Public Security Bureau,Beijing 100192, China
  • Online:2017-07-25 Published:2018-07-25

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摘要： 鉴于农业生产中大量使用季铵盐类农药造成的环境水污染问题,本文应用固相萃取与扫集-胶束电泳(Sweeping-MEKC)相结合的方法分析鱼塘水中的百草枯、敌草快和野燕枯3种季铵盐类除草剂。考察了缓冲液的浓度、pH值、十二烷基磺酸钠(SDS)浓度、有机添加剂种类及浓度、分离电压及其进样时间等对分离检测的影响,优化的电泳分析条件为:缓冲液为pH2.6的50 mmol/L磷酸盐缓冲液(含体积分数20%的乙腈),40 mmol/L十二烷基磺酸钠,6.895 kPa压力进样160 s,分离电压为-22 kV,紫外检测波长为198 nm,柱温为20 ℃。含季铵盐除草剂的鱼塘水经过Oasis WCX固相萃取柱富集后在上述优化电泳条件下进行分析,百草枯、敌草快及野燕枯的检出限(LOD)(S/N=3)分别为0.07,0.05 和0.02 μg/L,线性范围分别为0.2～100、0.15～100和0.05～100 μg/L;加样回收率为89.3%～107.1%,相对标准偏差为4.5%～11.4%。该方法灵敏度高,可实际应用于鱼塘水中季铵盐类除草剂农药残留分析。

关键词: 毛细管电泳, 扫集胶束, 鱼塘水, 固相萃取, 季铵盐类除草剂

Abstract: As great quantities of quaternary ammonium herbicides were used in agricultural production. In this article, conditions have been optimized for simultaneous determination of paraquat (PQ)、diquat (DQ) and difenzoquat(DF)by sweeping-MEKC with diode array detector (DAD) after their preconcentration by solid phase extraction(SPE). The influence of concentration of buffer,pH,concentration of SDS and organic modifier,separation voltage and injection time on the separation of quaternary ammonium herbicides were studied. An optimal separation condition was obtained by using background buffer containing 40 mmol/L SDS,50 mmol/L NaH2PO4 and 20% acetonitrile at pH2.6 with 20 ℃,the separation voltage at -22 kV,the sample injection time for 160 s at 6.895 kPa and 198 nm detection. The calibration curves showed good linearities in the range of 0.2~100 μg/L for paraquat,0.15~100 μg/L for diquat and 0.05~100 μg/L for difenzoquat,the limits of detections(S/N=3)for PQ, DQ and DF were 0.07, 0.05 and 0.02 μg/L respectively. The relative recoveries of the three quaternary ammonium herbicides ranged from 89.3% to 107.1% with relative standard deviation ranging from 4.5% to 11.4%. The method can be applied in the detection of quaternary ammonium herbicides in the agricultural pond water.

Key words: capillary electrophoresis, Sweeping-MEKC, pond water, solid phase extraction, quaternary ammonium herbicides

中图分类号: 

  • O658.2
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