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高效液相色谱-串联质谱法测定水、沉积物和土壤中的四溴双酚A及其溴化衍生物

Determination of tetrabromobisphenol A and its brominated derivatives in water, sediment and soil by high performance liquid chromatography-tandem mass spectrometry.

作者信息

Xie Hui, Xu Yuxin, Sun Fengxia, Li Jinling, Liu Ruiyuan

机构信息

College of Resources and Environment, Shandong Agricultural University, Taian, 271018, China.

出版信息

Anal Sci. 2023 Nov;39(11):1875-1888. doi: 10.1007/s44211-023-00393-7. Epub 2023 Jul 17.

Abstract

Tetrabromobisphenol A (TBBPA) was typical brominated flame retardant and potential environmental endocrine disruptor, and it had persistence, bioaccumulation and chronic toxicity. Simultaneous determination of ultra-trace TBBPA, tribromobiphenol A (tri-BBPA), dibromobiphenol A (di-BBPA), monobromobisphenol A (mono-BBPA) and bisphenol A (BPA) was developed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS), the parent ion charge ratios (m/z) had been optimized. The linear range was wider and the limit of detection was (LOD) 0.09 ~ 0.21 ng mL, which could detect trace pollutants. The extraction efficiency was improved by optimizing the parameters, HLB cartridge was used in the water sample by solid phase extraction (SPE), the recovery rates in water samples were over 80.28% with three concentration levels, the relative standard deviations (RSD) were less than 7.12%, and the minimum detection limit of the method was 0.90 ~ 2.10 × 10 ng mL. Soil and sediment samples were extracted by accelerated solvent extraction (ASE), the recovery rates in soil and sediment were over 79.40% and 75.65%, the minimum detection limit was 0.0225 ~ 0.0525 ng g, RSD was less than 7.19%. The proffered method was successfully utilized to detect actual samples, the residue of di-BBPA and mono-BBPA are detected in Naihe River and Shuxi River in Tai'an City, residue of di-BBPA and mono-BBPA was detected in the soil, and there was low residual amount of di-BBPA, mono-BBPA and BPA in the sediment of Shuxi River.

摘要

四溴双酚A(TBBPA)是典型的溴化阻燃剂和潜在的环境内分泌干扰物,具有持久性、生物累积性和慢性毒性。采用高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定超痕量的四溴双酚A(TBBPA)、三溴双酚A(tri-BBPA)、二溴双酚A(di-BBPA)、单溴双酚A(mono-BBPA)和双酚A(BPA),对母离子荷质比(m/z)进行了优化。线性范围较宽,检测限(LOD)为0.09~0.21 ng/mL,能够检测痕量污染物。通过优化参数提高了萃取效率,采用HLB柱对水样进行固相萃取(SPE),三个浓度水平的水样加标回收率均超过80.28%,相对标准偏差(RSD)小于7.12%,方法最低检测限为0.90~2.10×10 ng/mL。土壤和沉积物样品采用加速溶剂萃取(ASE),土壤和沉积物中的加标回收率分别超过79.40%和75.65%,最低检测限为0.0225~0.0525 ng/g,RSD小于7.19%。该方法成功应用于实际样品检测,在泰安市奈河和梳洗河检测到二溴双酚A和单溴双酚A的残留,在土壤中检测到二溴双酚A和单溴双酚A的残留,梳洗河沉积物中二溴双酚A、单溴双酚A和双酚A的残留量较低。

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