干旱区生态环境知识资源中心(Arid): 高效液相色谱/质谱法测定土壤中10种磺酰脲类除草剂多残留

Arid

	高效液相色谱/质谱法测定土壤中10种磺酰脲类除草剂多残留
其他题名	Determination of Ten Sulfonylurea Herbicides in Soil Samples by Liquid Chromatography with Electrospray Ionization Mass Spectrometric Detection
	叶贵标; 张微; 崔昕; 潘灿平; 江树人
ISSN	0253-3820
出版年	2006
卷号	34 期号:9 页码:1207-1212
中文摘要	建立了高效液相色谱/质谱法(HPLC-MS)同时检测土壤中10种磺酰脲类除草剂多残留量的方法.样品在磷酸缓冲液(pH值7.8):甲醇(8∶2,V/V)中经超声波萃取,提取液直接经固相萃取小柱净化,采用 HPLC-ESI(+)-MS 进行定性定量分析.比较了Cleanert C18,Cleannert HXN 和Oasis HLB 3种SPE商品柱的净化效果, 结果表明 Cleanert C18和Cleannert HXN柱的净化效果和回收率均较好.10种磺酰脲类农药的液相色谱分离在乙腈-甲醇-水(0.2%冰醋酸)梯度洗脱下完成,10个化合物的保留时间在10～16 min.10种磺酰脲类除草剂在0.1～10.0 mg/L范围内线性良好, 相关系数均在0.9964～0.9989之间;相对标准偏差在0.99%～4.26%之间.在0.01～1.0 mg/kg添加水平范围内,平均添加回收率在80.2%～104.5%之间(除苯磺隆).本方法中10种磺酰脲类除草剂在土壤中的检出限为0.6～3.5 mug/kg之间.
英文摘要	A multi-residue method has been developed for the confirmation and quantitation of ten sulfonly-lurea herbicides including nicosulfuron, thifensulfuron-methyl, metsulfuron-methyl, sulfometuron-methyl,chlorsulfuron, ethametsulfuron-methyl, tribenuron, bensulfuron-methyl, pyrazosulfuron-ethyl and chlorimuron-ethyl in soil. Samples were extracted from soil with methanol- phosphate buffer (2:8, V/V) (pH7. 8) underultrasonic bath. Then the extracts were brought to pH 2.5 with 85% H3PO+ and passed under vacuum througha solid-phase cartridge. Different types of sorbents were evaluated; silla-based Cleanert C)8 and two polymericsorbents, namely Oasis HLB and Cleanert HXN. The best results were obtained with Cleanert C18, and wasperformed.by high performance liquid chromatography (HPLC)-electrospray mass spectrometry(LC-ESI-MS)instrumentation equipped with ion trap mass filter. The HPLC column used.was a 4. 6 mm x250 mm XDB Ci8column, 5 jjum particle size. The mobile phase was acetonitrile-methanol-0.2% acetic acid. The elution gradient was as follows: the mobile phase started with 10% of acetonitrile and 10% methanol, which was increasedlinearly to 45% in 14 min, to 48% in the next 2 min and then returned to initial conditions in 2 min.Theicolumn was equilibrated for 5 min. The column temperature was kept at 30X1 and flow rate was 1. 0 mL/min. The retention times of 10 herbicides were between 10-16 min. The ten sulfonylurea compounds above mentioned were measured in fortified soil at 0.01 -1.0 mg/kg levels. Average recoveries were in the range of 80.2% -104.5% with relative standard deviations (RSDs) of 0.02% -14.9%. The limit of detection (LOD) was 0.6 -3.5 jig/kg.
中文关键词	磺酰脲类除草剂 ; 土壤 ; 多残留 ; 高效液相色谱电喷雾质谱 ; 固相萃取
英文关键词	Sulfonylurea herbicides soil multi-residue liquid chromatography-electrometry ionization-mass spectrometry solid phase extraction
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY MULTIDISCIPLINARY
WOS研究方向	Chemistry
CSCD记录号	CSCD:2434869
来源机构	中国农业大学
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/219616
作者单位	中国农业大学理学院, 北京 100094, 中国
推荐引用方式 GB/T 7714	叶贵标,张微,崔昕,等. 高效液相色谱/质谱法测定土壤中10种磺酰脲类除草剂多残留[J]. 中国农业大学,2006,34(9):1207-1212.
APA	叶贵标,张微,崔昕,潘灿平,&江树人.(2006).高效液相色谱/质谱法测定土壤中10种磺酰脲类除草剂多残留.,34(9),1207-1212.
MLA	叶贵标,et al."高效液相色谱/质谱法测定土壤中10种磺酰脲类除草剂多残留".34.9(2006):1207-1212.