加速溶剂萃取-气相色谱-串联质谱法测定松针中16种有机氯农药残留方法的中心组合设计优化
Optimization of GC-MS/MS Determination of Residual Amounts of 16 Organochlorine Pesticides in Pine Needle with Accelerated Solvent Extraction Based on Design-Expert
摘 要
采用加速溶剂萃取-气相色谱-串联质谱法测定松针中16种有机氯农药的残留量,并对萃取条件进行了优化.在气相色谱分离中用DB-5MS石英毛细管柱为固定相,在质谱分析中采用总离子扫描监测模式.16种有机氯农药在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.3~2.8 μg·L-1之间.方法用于松针样品分析,加标回收率在80.9%~99.2%之间,测定值的相对标准偏差(n=7)在2.9%~8.4%之间.
加速溶剂萃取
有机氯农药
松针
GC-MS/MS
Accelerated solvent extraction
Organochlorine pesticides
Pine needle
Abstract
GC-MS/MS was applied to the determination of residual amounts of 16 organochlorine pesticides in pine needle with accelerated solvent extraction.Extraction conditions of accelerated solvent extraction were optimized.The DB-5MS quartz capillary chromatographic column was used for GC separation and the total ion current monitoring mode were adopted in MS determination.Linear relationships between values of peak area and mass concentration of the 16 organochlorine pesticides were kept in definite ranges.Detection limits (3S/N) found were ranged from 0.3 to 2.8 μg·L-1.The proposed method was applied to the analysis of samples of pine needle,giving values of recovery and RSD′s (n=7) in the ranges of 80.9%-99.2% and 2.9%-8.4%,respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201508001
所属栏目 试验与研究
基金项目 国家自然科学基金(21163006);内蒙古科技支撑项目(20110506);内蒙古自治区科技计划项目(20120438);内蒙古科技创新基金(2011CXJJN01)
收稿日期 2014/8/21
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备注侯德坤(1979-),男,山东青州人,博士研究生,研究方向为环境地球化学.
引用该论文: HOU De-kun,HE Jiang,KHURELDAVAA Otgonbayar,ZHANG Fu-jin,ZHANG Xin-xin,ZHANG Min,ZHANG Ting-yu,YAO Yi-ping. Optimization of GC-MS/MS Determination of Residual Amounts of 16 Organochlorine Pesticides in Pine Needle with Accelerated Solvent Extraction Based on Design-Expert[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(8): 1049～1056
侯德坤,何江,呼日乐达瓦,张福金,张昕欣,张敏,张婷瑜,姚一萍. 加速溶剂萃取-气相色谱-串联质谱法测定松针中16种有机氯农药残留方法的中心组合设计优化[J]. 理化检验－化学分册, 2015, 51(8): 1049～1056
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【4】岳瑞生.《关于就某些持久性有机污染物采取国际行动的斯德哥尔摩公约》及其谈判背景[J].世界环境,2001(1):24-28．
【5】ALONSO-HERNANDEZ C M,MESA-ALBERNAS M,TOLOSA I.Organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in sediments from the Gulf of Batabanó,Cuba[J].Chemosphere,2014,94:36-41．
【6】CHENG Hai-rong,LIN Tian,ZHANG Gan,et al.DDTs and HCHs in sediment cores from the Tibetan Plateau[J].Chemosphere,2014,94:183-189．
【7】LI Yuan-yuan,LIN Tian,QIN Yan-wen,et al.Distribution and sources of organochlorine pesticides in sediments of the Xiangjiang River,south-central China[J].Environ Monit Assess,2013,185:8861-8871．
【8】OZCAN S,AYDIN M E,TOR A.Chromatographic separation and analytic procedure for priority organic pollutants in urban air[J].Clean-Soil Air Water,2008,36(12):969-977．
【9】ZHANG Li-fei,DONG Liang,YANG Wen-long,et al.Passive air sampling of organochlorine pesticides and polychlorinated biphenyls in the Yangtze River Delta,China:concentrations,distributions,and cancer risk assessment[J].Environ Pollut,2013,181:159-166．
【10】SHEN Zhi-gang,HE Ze-ying,WANG Peng,et al.Low-density magnetofluid dispersive liquid-liquid microextraction for the fast determination of organochlorine pesticides in water samples by GC-ECD[J].Anal Chim Acta,2013,793:37-43．
【11】YUAN Lin-xi,QI Shi-hua,WU Xiao-guo,et al.Spatial and temporal variations of organochlorine pesticides (OCPs) in water and sediments from Honghu Lake,China[J].J Geochem Explor,2013,132:181-187．
【12】DEVIN L,CHAKRABORTY P,QI Shi-hong,et al.Selected organochlorine pesticides (OCPs) in surface soils from three major states from the northeastern part of India[J].Environ Monit Assess,2013,185(8):6667-6676．
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