CAJ | 학술논문

建立了土壤中8种羟基化多溴联苯醚( Hydroxylated polybrominated diphenyl ethers, 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9 min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0.23~1.21 ng/g。在5.0和50 ng/g 2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。
건립료토양중8충간기화다추련분미( Hydroxylated polybrominated diphenyl ethers, OH-PBDEs)적QuEChERS-초고효액상색보천련질보( UPLC-MS/MS)분석방법。양품전처리채용QuEChERS방법,토양양품용수침윤지후,이갑산화을정제취목표물,C18전료화정병기을이알( PSA)정화,C18색보주분리,을정화수제도세탈,다반응감측부리자모식소묘。재최가실험조건하,8충목표물재9 min내분리량호,병재2~200μg/L범위내선성량호,상관계수범위재0.9936~0.9990,검출한범위위0.23~1.21 ng/g。재5.0화50 ng/g 2개농도수평6차평행가표실험중,8충OH-PBDEs평균회수솔위73.2%~117.7%,상대표준편차위5.6%~19.7%。본방법조작간편,령민도고,괄용우대비량양품적쾌속분석。
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.