固相萃取-高效液相色谱法考察可溶性有机物对绿麦隆在小麦体内积累的影响
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摘要
[目的]建立了固相萃取-高效液相色谱法研究可溶性有机物对绿麦隆在小麦体内积累的影响。[方法]采用乙腈-水为提取溶剂,通过固相萃取Sep-pak C_(18)柱分离和混合模式的GCC-SAX-PSA串联柱净化,反相高效液相色谱法定量分析了2种可溶性有机物(DOM)对绿麦隆在小麦体内积累的影响。[结果]该方法最小检出限为2×10-10g,最低检出质量分数为0.05 mg/kg,小麦叶片和根系中绿麦隆添加回收率为85.7%、92.4%,变异系数0.2%、2.8%。[结论]研究发现绿麦隆施药质量分数较低(5 mg/kg)时,可溶性有机物可以降低绿麦隆在小麦幼苗体内的含量,可降低其生物毒性;当施药质量分数较高(10、25 mg/kg)时,可溶性有机物使绿麦隆在小麦幼苗体内的含量增高,增大其生物毒性。来源于稻草的可溶性有机物对小麦幼苗吸收绿麦隆的影响强于来源于污泥的可溶性有机物,并且随可溶性有机物浓度的增高,影响增大。
[Aims] An improved reversed phase high performance liquid chromatographic method for the determination of chlorotoluron in leave and root of wheat was established. [Methods] The method involved an initial extraction of the wheat with acetonitrile-water. Implementation of a mixed-mode solid-phase extraction Sep-pak C_(18) and GCC-SAX-PSA SPE cartridges was discussed as a promising approach for wheat clean-up. The effect of dissolved organic matter on chlorotoluron accumulation in wheat seedling was studied. [Results] The chlorotoluron content was determined by high performance liquid chromatography with UV detection. Recoveries of chlorotoluron was 85.7-92.4% and with coefficient of variability of 0.2-2.8%. The minimum detectable amount of chlorotoluron was 2 ×10-10 g, and minimum detectable concentration was 0.05 mg/kg. [Conclusions] The results showed that treatment dissolved organic matter induced decrease in chlorotoluron content of wheat seedling with the initial concentration(5 mg/kg) of chlorotoluron in soil and increase in chlorotoluron content of wheat seedling with the initial concentration(10-25 mg/kg) of chlorotoluron in soil. The effect of soluble organic matter from straw on the absorption of chlorotoluron in wheat seedlings was stronger than that from sludge, and the effect increased with the increase of the concentration of soluble organic matter.
[Aims] An improved reversed phase high performance liquid chromatographic method for the determination of chlorotoluron in leave and root of wheat was established. [Methods] The method involved an initial extraction of the wheat with acetonitrile-water. Implementation of a mixed-mode solid-phase extraction Sep-pak C_(18) and GCC-SAX-PSA SPE cartridges was discussed as a promising approach for wheat clean-up. The effect of dissolved organic matter on chlorotoluron accumulation in wheat seedling was studied. [Results] The chlorotoluron content was determined by high performance liquid chromatography with UV detection. Recoveries of chlorotoluron was 85.7-92.4% and with coefficient of variability of 0.2-2.8%. The minimum detectable amount of chlorotoluron was 2 ×10-10 g, and minimum detectable concentration was 0.05 mg/kg. [Conclusions] The results showed that treatment dissolved organic matter induced decrease in chlorotoluron content of wheat seedling with the initial concentration(5 mg/kg) of chlorotoluron in soil and increase in chlorotoluron content of wheat seedling with the initial concentration(10-25 mg/kg) of chlorotoluron in soil. The effect of soluble organic matter from straw on the absorption of chlorotoluron in wheat seedlings was stronger than that from sludge, and the effect increased with the increase of the concentration of soluble organic matter.
引文
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[14]BALINOVA A,MLADENOVA R,SHTEREVA D.Solid-phase Extraction on Sorbents of Different Retention Mechanisms Followed by Determination by Gas Chromatography Mass Spectrometric and Gas Chromatography-electron Capture Detection of Pesticide Residues in Crops[J].Journal of Chromatography A,2007,1150:136-144.
[2]徐鹏,范洁,鲁炳闻,等.绿麦隆农药纯度标准物质的定值及不确定度评定[J].农药,2013,52(9):660-663.
[3]庄占兴,于庆利,韩书霞,等.绿麦隆与莠去津混用防除玉米田杂草[J].农药,1996,29(2):63.
[4]张国聚,陈国参.除草剂混用原理与应用技术[M].北京:中国农业出版社,1999:40-48.
[5]吕文彦,娄国强.苯磺隆、绿麦隆混用最佳配比防除麦田杂草技术研究[J].河南农业大学学报,2007,41(1):80-81.
[6]曹志磊,俞花美,葛成军,等.可溶性有机物对土霉素在土壤中吸附-解吸的影响[J].热带作物学报,2018,39(4):825-831.
[7]刘阳,张磊.两种海源可溶性有机物对汞在沉积物中吸附特性的影响[J].环境化学,2015,34(2):247-253.
[8]ZHU Wen-zhuo,ZHANG Jing,YANG Gui-peng.Mixing Behavior and Photobleaching of Chromophoric Dissolved Organic Matter in the Changjiang River Estuary and the Adjacent East China Sea[J].Journal of Estuarine,Coastal and Shelf Science,2018,207(31):422-434.
[9]李丹,何小松,高如泰,等.紫外-可见光谱研究堆肥水溶性有机物不同组分演化特征[J].中国环境科学,2016,36(11):3412-3421.
[10]宋宁慧,单正军.水溶性有机物对绿麦隆胁迫下小麦幼苗生物利用性和毒性的影响[J].环境科学研究,2012,25(4):460-466.
[11]KAUSHIK M,NEERA S.Effect of Soil Amendments on Sorption and Mobility of Metribuzin in Soils[J].Chemosphere,2007,66:630-637.
[12]张馨予,液相色谱法测定玉米和土壤中绿麦隆的方法[J].中国农学通报,2016,32(31):138-142.
[13]孙斌慧,李常平.高效液相色谱法分析40%胶悬剂中绿麦隆和阿特拉津[J].农药,1991,30(2):23-24.
[14]BALINOVA A,MLADENOVA R,SHTEREVA D.Solid-phase Extraction on Sorbents of Different Retention Mechanisms Followed by Determination by Gas Chromatography Mass Spectrometric and Gas Chromatography-electron Capture Detection of Pesticide Residues in Crops[J].Journal of Chromatography A,2007,1150:136-144.