The purpose of this study was to develop a novel and sensitive method for the analysis of carbazole and polyhalogenated carbazoles (PHCs) in sediment using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Briefly, 5.0 g of freeze-dried sediment samples were extracted with dichloromethane using pressurized liquid extraction (PLE). The extract was purified with Florisil solid phase extraction cartridge, filtered through 0.22 µm polytetrafluoroethylene filter using a glass syringe, followed by LC-MS/MS analysis. Besides parameters for LC-MS/MS analysis, sample preparation procedures (including solvents for PLE, sorbents for cleanup, and filters for sample filtration) were optimized. The limits of detection and limits of quantification of target compounds were in the ranges of 3.0 × 10⁻³ to 0.22 ng g⁻¹ dry weight (d.w.) and 1.0 × 10⁻² to 0.75 ng g⁻¹ d.w., respectively. The recoveries of target compounds in the spiked sediments at 2.0 ng g⁻¹ d.w. and 10 ng g⁻¹ d.w. were 64.8–91.8% and 70.9–124.7%, respectively, with relative standard deviations being less than 13.2%. Except that 36-BCZ had positive matrix effects of 63.3%, the sediment matrices generally displayed low or medium negative matrix effects on the other target compounds during LC-MS/MS analysis. The developed method was applied in the analysis of carbazoles and PHCs in sediment samples from Jiulong River, Fujian, China and all the target compounds were detected in the samples.

这项研究的目的是开发一种新型，灵敏的方法，使用超高效液相色谱-串联质谱（UPLC-MS / MS）分析沉积物中的咔唑和多卤代咔唑（PHC）。简要地，使用加压液体萃取（PLE）用二氯甲烷萃取5.0 g冻干的沉积物样品。萃取物用Florisil固相萃取柱纯化，使用玻璃注射器通过0.22 µm聚四氟乙烯过滤器过滤，然后进行LC-MS / MS分析。除了用于LC-MS / MS分析的参数外，还优化了样品制备程序（包括用于PLE的溶剂，用于净化的吸附剂和用于样品过滤的过滤器）。目标化合物的检出限和定量限在3.0×10 ^-3的范围内至干重（dw）为0.22 ng g ^-1 dw和1.0 ng g ^-1 dw为1.0×10 ^-2 dg ^-1 dw。加标沉积物中2.0 ng g ^-1 dw和10 ng g ^-1 dw的目标化合物的回收率分别为64.8–91.8％和70.9–124.7％，相对标准偏差小于13.2％。除36-BCZ具有63.3％的正基质效应外，在LC-MS / MS分析过程中，沉积物基质对其他目标化合物通常表现出低或中等的负基质效应。该方法用于福建省九龙江沉积物样品中咔唑和PHC的分析，样品中所有目标化合物均被检测到。