College of Environment, Zhejiang University of Technology, Hangzhou, 310014, China.
Ecology and Environment Bureau of Qiannan, Guizhou, 558300, China.
Environ Sci Pollut Res Int. 2023 Aug;30(36):86255-86267. doi: 10.1007/s11356-023-28535-4. Epub 2023 Jul 5.
A precise analytical method based on QuEChERS has been proposed for the concurrent determination of 11 polyhalogenated carbazoles (PHCZs), benzocarbazole (BZCZ), and 9H-carbazoles (CZ). The quantification was confirmed by gas chromatography using triple quadrupole tandem mass spectrometry (Shimadzu GC-MS/MS-TQ8040) and gas chromatography coupled mass spectrometry (Agilent 7890A-5973 GC-MS). The developed method was validated by testing the following parameters: linearity, instrument limit of detection (LOD), instrument limit of quantification (LOQ), method limit of detection (MLD), method limit of quantification (MLQ), matrix effect (ME), accuracy, and precision. All compounds showed good linearity in the range of 0.005-0.2 μg/mL with correlation coefficients higher than 0.992. The method demonstrated satisfactory recoveries (ranging from 71.21 to 105.04%) for most of the compounds with relative standard deviation precision (RSD) < 10.46%, except 3-BCZ (Recovery = 67.53%, RSD = 2.83%). The values of LOD and LOQ varied from 0.05 to 0.24 ng and 0.14 to 0.92 ng, respectively, while those of MLD and MLQ ranged from 0.02 to 0.12 ng/g wet weight (ww) and 0.07 to 0.45 ng/g ww, respectively. The developed method represents a reliable tool for the routine analysis of PHCZ congeners in invertebrate animals.
一种基于 QuEChERS 的精确分析方法已被提出，用于同时测定 11 种多卤代咔唑（PHCZs）、苯并咔唑（BZCZ）和 9H-咔唑（CZ）。通过三重四极杆串联质谱（岛津 GC-MS/MS-TQ8040）和气相色谱-质谱联用（安捷伦 7890A-5973 GC-MS）对定量进行了确认。通过测试以下参数对所开发的方法进行了验证：线性、仪器检测限（LOD）、仪器定量限（LOQ）、方法检测限（MLD）、方法定量限（MLQ）、基质效应（ME）、准确度和精密度。所有化合物在 0.005-0.2μg/mL 范围内均表现出良好的线性，相关系数均高于 0.992。对于大多数化合物，该方法的回收率（范围为 71.21%至 105.04%）令人满意，相对标准偏差精度（RSD）<10.46%，除 3-BCZ（回收率=67.53%，RSD=2.83%）外。LOD 和 LOQ 的值分别在 0.05 至 0.24ng 和 0.14 至 0.92ng 之间，而 MLD 和 MLQ 的值分别在 0.02 至 0.12ng/g 湿重（ww）和 0.07 至 0.45ng/g ww 之间。该方法是一种用于常规分析无脊椎动物中 PHCZ 同系物的可靠工具。
