溶剂萃取-气相色谱-三重四极杆串联质谱法测定水体和土壤中6种邻苯二甲酸酯

Determination of Six Phthalic Acid Esters in Water and Soil Samples by Gas Chromatography-Tandem Mass Spectrometry with Solvent Extraction Method

采用溶剂萃取分离法提取水体和土壤中的邻苯二甲酸酯(PAEs),优化了提取剂及提取步骤,建立了简便、快速、高通量测定水体和土壤样本中6种PAEs的气相色谱-三重四极杆串联质谱法(GC-MS/MS)。结果表明,水样和土样的最佳萃取剂分别为正己烷和乙腈,提取容器和涡旋时间是影响PAEs回收率的关键因素,离心温度、超声时间、提取次数和氮吹等步骤对PAEs回收率影响较小。在最优条件下,在0.5~100μg/L范围内6种PAEs的峰面积与浓度线性关系良好(相关系数R^(2)>0.9926)。选取了1种河水和2种土壤基质,分别在3个加标水平和2个加标水平下验证了提取方法的准确度和精密度,6种PAEs在水体和土壤中的平均回收率分别为85.6%~112.5%和94.3%~114.3%,相对标准偏差均小于10%。方法适用于水体和土壤等环境样本中PAEs残留的监测。

Herein,a simple,fast and high-throughput method was established for the simultaneous determination of six phthalic acid esters(PAEs)in water and soils using the optimized solvent extraction methods,followed by gas chromatography-tandem mass spectrometry(GC-MS/MS)detection.The results indicated that n-hexane and acetonitrile were the best solvents for extraction in water and soil samples,respectively.The extraction container and vortex time were the main factors affecting the recoveries of PAEs in above samples,while centrifuge temperature,ultrasonic time,extraction time,nitrogen blowing and other steps involved in the extraction process had little effect on the recoveries of PAEs.Under the optimal conditions,good linearity(R^(2) value>0.9926)was observed at concentration range of 0.5-100μg/L for the 6 PAEs determined by GC-MS/MS.Three types of environmental samples,i.e.,one water and two soils were selected to verify the accuracy and precision of the method at three and two levels,respectively.The average triplicate recoveries of PAEs in spiked water and soils ranged from 85.6%to 112.5%and 94.3%to 114.3%,respectively,and the relative standard deviations(RSDs)were less than 10%for all of the recovery tests.The method is suitable for the monitoring of PAEs residues in environmental samples such as water and soils.