超高效液相色谱-质谱法检测土壤中的羟基化多溴联苯醚  

Determination of Hydroxylated Polybrominated Diphenyl Ethers in Soils by QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：徐能斌[1] 钱飞中[1] 冯加永[1] 汪晟乐[1] 洪正昉[2] 徐立红 陈钟佺[1] 

机构地区：[1]宁波市环境监测中心,宁波315012 [2]浙江省环境监测中心,杭州310012 [3]绍兴市环境监测中心,绍兴312000

出　　处：《分析化学》2015年第2期251-256,共6页Chinese Journal of Analytical Chemistry

基　　金：国家高技术研究发展计划(No.2011AA060603);环保部科研公益性行业专项(No.201209016);宁波市自然科学基金(No.2011A610087)资助~~

摘　　要：建立了土壤中8种羟基化多溴联苯醚（Hydroxylated polybrominated diphenyl etllers，OH—PBDEs）的QuEChERS-超高效液相色谱串联质谱（UPLC—MS／MS）分析方法。样品前处理采用QuEChERS方法，土壤样品用水浸润之后，以甲酸和乙腈提取目标物，C18填料和正丙基乙二胺（PSA）净化，C18色谱柱分离，乙腈和水梯度洗脱，多反应监测负离子模式扫描。在最佳实验条件下，8种目标物在9min内分离良好，并在2～200μg／L范围内线性良好，相关系数范围在0．9936～0．9990，检出限范围为0．23—1．21ng／g。在5．0和50ng／g2个浓度水平6次平行加标实验中，8种OH—PBDEs平均回收率为73．2％-117．7％，相对标准偏差为5．6％-19．7％。本方法操作简便，灵敏度高，适用于大批量样品的快速分析。An QuEChERS-UPLC-MS/MS method was developed for the simultaneous determination of eight hydroxylated polybrominated diphenyl ethers（OH-PBDEs） in soil samples. After being mixed with 10 mL of water, the sample was extracted with acidified acetonitrile, cleaned up by ClS and primary secondary amine （PSA）. The separation of eight OH-PBDEs was performed on a C18 column using gradient elution of acetonitrile and water as mobile phase within 9 min. The OH-PBDEs were analyzed under the multiple- reaction monitoring （MRM） mode with negative electrospay ionization. Under the optimal conditions, the calibration curves were linear well in the range of 2- 200 μg/L with correlation coefficients ranging from 0. 9936 to 0.9990, and the limits of detection of eight OH-PBDEs were in the range of 0.23-1.21 ng/g. At the spiked levels of 5.0 and 50 ng/g, the average spiked recoveries for eight OH-PBDEs were between 73.2% and 117.7%, method is simple and with the relative standard derivations （RSDs） from 5.6% to 19.7%. The developed sensitive, and suitable for the rapid analysis of large quantities of samples.

关 键 词：羟基化多溴联苯醚 土壤 超高效液相色谱-质谱法 

分 类 号：X833[环境科学与工程—环境工程] O657.63[理学—分析化学]