摘要
以地表水环境质量标准严格控制的特定项目为依据，建立了直接进样-高效液相色谱-串联质谱同时测定水中13种化学性质差异较大的有机污染物的分析方法，这13种有机污染物为乐果、敌敌畏、敌百虫、对硫磷、甲基对硫磷、马拉硫磷、内吸磷、丙烯酰胺、苯胺、联苯胺、甲萘威、微囊藻毒素-LR、阿特拉津。水样经0.22μm 尼龙66滤膜过滤后，采用 Kromasil 100-5 C18柱（150 mm×2.1 mm，5μm）分离，以甲醇-0.01％甲酸水溶液为流动相进行梯度洗脱，流速0.5 mL／min，柱温40℃，电喷雾正离子模式（ESI＋）电离，多反应监测模式（MRM）进行检测，外标法定量。13种化合物的浓度与其峰面积在一定浓度范围内均呈现良好的线性关系（ r≥0.9995），方法检出限为0.02～0.1μg／L。测定低、中、高浓度的加标样品，13种化合物的相对标准偏差为0.5％～5.0％（ n＝6），实际样品加标平均回收率为81.2％～112％。此方法灵敏度高、干扰小、分析速度快，可适用于地表水、地下水中这13种有机污染物的同时分析。
On the basis of environmental quality standards for surface water,a sensitive and simple method was developed for the simultaneous determination of 13 organic pollutants, including dimethoate,dichlorvos,trichlorfon,parathion,methyl parathion,malathion,deme-ton,acrylamide,aniline,benzidine,carbaryl,Microcystin-LR and atrazine in water samples by high performance liquid chromatography-tandem mass spectrometry（ HPLC-MS/MS）combined with direct injection. The water samples were filtered through 0. 22 μm of microfiltration mem-brane. With methanol-0. 01% formic acid as mobile phase,the separation was performed on a Kromasil 100-5 C18 column（150 mm×2. 1 mm,5 μm）in gradient elution. The flow rate was 0. 5 mL/min. The column temperature was 40 ℃. The samples were detected by multiple reac-tion monitoring（ MRM ） mode with positive electro spray ionization. The organic pollutants were quantified by external standard method. The calibration curves of the organic pollutants show good linearity in suitable ranges with correlation coefficients（ r）over 0. 999 5. The detec-tion limits of organic pollutants in samples ranged from 0. 02 μg/L to 0. 1 μg/L. The relative standard deviations of organic pollutants were 0. 5%-5. 0%（ n=6）. The average recoveries of the 13 organic pollutants spiked in water samples ranged from 81. 2% to 112%. The method has been proven to be sensitive,rapid and with little interference. It is suitable for the determina-tion of the 13 organic pollutants simultaneously in the surface and underground waters.
出处
《色谱》
CAS
CSCD
北大核心
2015年第7期740-745,共6页
Chinese Journal of Chromatography
关键词
高效液相色谱-串联质谱法
有机污染物
水样
直接进样
high performance liquid chromatography-tandem mass spectrometry（ HPLC-MS/MS）
organic pollutants
water samples
direct injection
