干旱区生态环境知识资源中心(Arid): 固相萃取-超高效液相色谱-串联质谱法同时检测地表水中的35种农药及降解产物

Arid

	固相萃取-超高效液相色谱-串联质谱法同时检测地表水中的35种农药及降解产物
其他题名	Simultaneous Determination of Thirty-five Pesticides and Transformation Products in Surface Water Using Solid Phase Extraction Combined with Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry
	孙静; 徐雄; 李春梅; 罗茜; 王东红; 王子健
来源期刊	分析化学
ISSN	0253-3820
出版年	2015
卷号	43 期号:8 页码:1145-1153
中文摘要	采用固相萃取(SPE)-超高效液相色谱串联质谱(UPLC-MS/ MS)技术,建立了同时测定环境水样中痕量浓度多极性的35种高关注农药及转化产物的方法。优化的前处理方法为:串联HLB和活性炭小柱用于富集水样,10 mL乙腈为HLB柱洗脱溶剂,10 mL 20 mmol/ L乙酸铵-甲醇作为活性炭柱的洗脱溶剂,将洗脱溶液混合、浓缩、溶剂转化和定容,定容溶剂为10 mmol/ L乙酸铵的乙腈-水的混合溶液(1:1, V / V)。流动相分别为5 mmol/ L甲酸铵-甲酸缓冲溶液(pH 3. 5)和乙腈进行UPLC色谱分离,质谱用多反应监测(MRM)模式进行分析测定。实验结果表明,目标物在0. 5 ~200 mug/ L含量范围内线性良好(R~2≥0. 9802),检出限范围为0. 01 ~0. 8 ng/ L,回收率在60% ~120%之间。本研究构建的SPE-UPLC-MS/ MS方法灵敏可靠,可用于对地表水中ng/ L级极性不同的多种农药及转化产物的测定。
英文摘要	A method based on solid phase extraction combined with ultra-performance liquid chromatographytandem mass spectrometry (SPE-UPLC-MS/ MS) was established for the simultaneous determination of thirtyfive pesticides and transformation products of high concern with different polarities at trace level in environmental waters. Under optimized conditions, tandem cartridges with Oasis HLB column and activated carbon were used for the enrichment of water samples. HLB column was eluted by 10 mL of acetonitrile, and activated carbon cartridge was eluted by 10 mL of methanol solution containing 20 mmol/ L ammonium acetate. The elution solvents were mixed, concentrated and reconstituted. Finally, the elution solvent was reconstituted with a mixed solution of acetonitrile and water (1:1, V / V) containing 10 mmol/ L ammonium acetate. The targets were separated by gradient elution with 5 mmol/ L ammonium formate buffer and acetonitrile as mobile phases, and detected by MS/ MS in the multi-reactions monitoring (MRM) mode. Under the experimental conditions, good linearity ranging from 0. 5-200 mug/ L was made (R~2≥0. 9802), and the limits of detection (LODs) were from 0. 01 ng/ L to 0. 8 ng/ L. Recoveries of most targets were 60% -120%. The SPE-UPLC- MS/ MS method established here is reliable and can be applied to determine ng/ L level of pesticides and transformation products with different polarities in surface water.
中文关键词	农药 ; 转化产物 ; 固相萃取 ; 超高效液相色谱-串联质谱法 ; 地表水
英文关键词	Pesticides Transformation products Solid phase extraction Ultra high performance liquid chromatography-tandem mass spectrometry Surface water
语种	中文
国家	中国
收录类别	CSCD
WOS类目	ENVIRONMENTAL SCIENCES
WOS研究方向	Environmental Sciences & Ecology
CSCD记录号	CSCD:5502590
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/232583
作者单位	中国科学院生态环境研究中心, 环境水质学国家重点实验室, 北京 100085, 中国
推荐引用方式 GB/T 7714	孙静,徐雄,李春梅,等. 固相萃取-超高效液相色谱-串联质谱法同时检测地表水中的35种农药及降解产物[J],2015,43(8):1145-1153.
APA	孙静,徐雄,李春梅,罗茜,王东红,&王子健.(2015).固相萃取-超高效液相色谱-串联质谱法同时检测地表水中的35种农药及降解产物.分析化学,43(8),1145-1153.
MLA	孙静,et al."固相萃取-超高效液相色谱-串联质谱法同时检测地表水中的35种农药及降解产物".分析化学 43.8(2015):1145-1153.