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

• • 上一篇    下一篇

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

PDF (PC)

210

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
[1] 王静, 刘铮铮. 固相萃取-液相色谱/紫外法测定地表水中百草枯和敌草快[J]. 中国环境监测, 2011, 27(4): 50-51.
[2] NEZ O, KIM J B, MOYANO E, et al. Analysis of the herbicides paraquat, diquat and difenzoquat in drinking water by micellar electrokinetic chromatography using sweeping and cation selective exhaustive injection[J]. Journal of Chromatography A, 2002, 961(1): 65-75.
[3] 李爱军, 王明泰, 牟峻, 等.食品中野燕枯残留量的测定[J]. 农药, 2007, 45(12): 842-844.
[4] ZHANG J Q, ZHAI C X, WANG F, et al. A bis(m-phenylene)-32-crown-10-based fluorescence chemosensor for paraquat and diquat[J]. Tetrahedron Letters, 2008, 49(34): 5009-5012.
[5] 石杰, 陈锦辉, 秦文华, 等. 尿中百草枯的快速检验[J]. 中国卫生检验杂志, 2006, 16(8): 943-944.
[6] GAO L, LIU J, WANG C, et al. Fast determination of paraquat in plasma and urine samples by solid-phase microextraction and gas chromatography-mass spectrometry[J]. Journal of Chromatography B, 2014, 944: 136-140.
[7] SAITO T, FUKUSHIMA T, YUI Y, et al. Monolithic spin column extraction and GC-MS for the simultaneous assay of diquat, paraquat, and fenitrothion in human serum and urine[J]. Analytical and Bioanalytical Chemistry, 2011, 400(1): 25-31.
[8] SUN B, CHEN Y. A simple and rapid method for detection of paraquat in human plasma by high-performance liquid chromatography[J]. International Journal of Clinical and Experimental Medicine, 2015, 8(10): 17067.
[9] SANTOS M S F, MADEIRA L M, ALVES A. Paraquat quantification in deposits from drinking water networks[J]. Analytical Methods, 2014, 6(11): 3791-3798.
[10] ZOU T, HE P, CAO J, et al. Determination of paraquat in vegetables using HPLC-MS-MS[J]. Journal of Chromatographic Science, 2015, 53(2): 204-209.
[11] 李捷, 杨方, 卢声宇, 等. 超高效液相色谱-电喷雾串联质谱法测定茶叶中敌草快和百草枯残留[J]. 分析试验室, 2014, 5:13.
[12] CAO H, KANG M, CHEN Z, et al. Determination of five quaternary ammonium compounds in foodstuffs using high performance liquid chromatography-tandem mass spectrometry[J].Analytical Methods, 2014, 6(13): 4790-4796.
[13] LANARO R, COSTA J L, CAZENAVE S O S, et al. Determination of herbicides paraquat, glyphosate, and aminomethylphosphonic acid in marijuana samples by capillary electrophoresis[J]. Journal of Forensic Sciences, 2015, 60(S1): 241-247.
[14] KUKUSAMUDE C, SRIJARANAI S, KATO M, et al. Cloud point sample clean-up and capillary zone electrophoresis with field enhanced sample injection and micelle to solvent stacking for the analysis of herbicides in milk[J]. Journal of Chromatography A, 2014, 1351: 110-114.
[15] LIU C, WANG P, SHEN Z, et al. pH-controlled quaternary ammonium herbicides capture/release by carboxymethyl-β-cyclodextrin functionalized magnetic adsorbents: mechanisms and application[J]. Analytica Chimica Acta, 2015, 901: 51-58.
[16] NEZ O, MOYANO E, GALCERAN M T.Capillary electrophoresis-mass spectrometry for the analysis of quaternary ammonium herbicides[J]. Journal of Chromatography A, 2002, 974(1-2): 243-255.
[17] 张庆庆, 孟品佳, 王燕燕, 等. 毛细管区带电泳场放大进样检测自来水中季铵盐类除草剂[J]. 刑事技术, 2016, 41(4): 265-269.
[18] BACIGALUPO M A, MERONI G, MIRASOLI M, et al. Ultrasensitive quantitative determination of paraquat:application to river, ground, and drinking water analysis in an agricultural area[J]. Journal of Agricultural and Food Chemistry, 2005, 53(2): 216-219.
[19] 张庆庆, 王燕燕, 孟品佳. 季铵盐类农药残留检测前处理研究进展[J]. 材料导报, 2014, 28(7): 85-89.
[20] ZHANG S, YANG X, YIN X, et al. Dispersive liquid-liquid microextraction combined with sweeping micellar electrokinetic chromatography for the determination of some neonicotinoid insecticides in cucumber samples[J]. Food Chemistry, 2012, 133(2): 544-550.
[21] YOUNG M S, JENKLNS K M. 河水中百草枯和敌草快的SPE和LC-MS分析方法[J].环境化学, 2004, 23(6): 722-723.
[22] 朱震海, 宣栋梁. 固相萃取-HPLC 法测定水中敌草快、百草枯[J]. 中国卫生检验杂志,2011, 21(9): 2154-2156.
[23] 陈静, 刘召金, 安保超, 等. 在线净化/固相萃取-高效液相色谱法测定饮用水和环境中的百草枯和敌草快[J]. 色谱, 2012, 30(10): 1068-1073.
[24] ZHOU Q, MAO J, XIAO J, et al. Determination of paraquat and diquat preconcentrated with N doped TiO2 nanotube solid phase extraction cartridge prior to capillary electrophoresis[J]. Analytical Methods, 2010, 2(8): 1063-1068.
[1] 张军文,李成思,卢永昌,史生辉. MEKC测定麻花艽中齐墩果酸和熊果酸含量[J]. 广西师范大学学报（自然科学版）, 2018, 36(1): 99-104.
[2] 李云荣, 吴昊, 田婷婷, 袁晋, 刘莉芳, 米伟, 常银霞, 杜黎明. 磁固相萃取快速测定环境水样中莠去津和扑草净[J]. 广西师范大学学报（自然科学版）, 2015, 33(4): 108-114.
[3] 郭利辉, 田一方, 梅晓芸, 张新爱, 陈冠华. 苯唑西林分子印迹聚合物的制备及其分子识别特性研究[J]. 广西师范大学学报（自然科学版）, 2015, 33(1): 86-92.
Viewed
Full text


Abstract

Cited
  Shared   
  Discussed   
No Suggested Reading articles found!
版权所有 © 广西师范大学学报（自然科学版）编辑部
地址：广西桂林市三里店育才路15号　邮编：541004
电话：0773-5857325　E-mail: gxsdzkb@mailbox.gxnu.edu.cn
本系统由北京玛格泰克科技发展有限公司设计开发