分析化学Issue(2)：251-256,6.DOI:10.11895/j.issn.0253-3820.140589
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
摘要
Abstract
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 C18 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%, with the relative standard derivations ( RSDs) from 5. 6% to 19. 7%. The developed method is simple and 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Key words
Hydroxylated polybrominated diphenyl ethers/Soils/Ultra performance liquid chromatography-tandem mass spectrometry引用本文复制引用
徐能斌,钱飞中,冯加永,汪晟乐,洪正昉,徐立红,陈钟佺..超高效液相色谱-质谱法检测土壤中的羟基化多溴联苯醚[J].分析化学,2015,(2):251-256,6.基金项目
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This work was supported by the National High Tech Research and Development Program (No.2011AA060603), the Special Fund for Envi-ronmental Scientific Research in the Public Interest (No.201209016) and the Ningbo City Natural Science Foundation (No.2011A610087) （ No.2011AA060603）
