Fu Qiang, Yao Dunfan, He Shuqing, Fang Yun, Wang Guowei, Li Jianhua, Xiao Chunqiao
Hubei Key Laboratory of Microbial Transformation and Regulation of Biogenic Elements, School of Environmental Ecology and Biological Engineering, Wuhan Institute of Technology, Wuhan, People's Republic of China.
School of Pharmacy, Xianning Medical College, Hubei University of Science and Technology, Xianning, People's Republic of China.
J Sep Sci. 2025 Jul;48(7):e70214. doi: 10.1002/jssc.70214.
Carbazole derivatives (CZDs) are an important class of nitrogen-containing heterocyclic compounds which have been widely used in photoelectric materials, dyes, medicine, supramolecules and other fields. The ecological risks of CZDs released into environment during the production and product utilization have gradually attracted people's attention. However, for the lack of analytical methods of CZDs in environment, the levels of CZDs entering the environment remain unclear. Herein, an analytical methodology for simultaneous measuring 13 CZDs associated with photoelectric materials in sediment samples has been established by using ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) in combination with a QuEChERS pretreatment technique. The parameters of the sample pretreatment and UHPLC-HRMS analysis were optimized. The established method was validated by evaluating its recovery, accuracy, matrix effect, limits of method detection (LODs), and so on. The instrument detection exhibits a linear response within concentration range of 1 to 1000 µg/L, and the LODs were ranged from 0.005 to 0.165 µg/kg. The average recoveries for the majority of CZDs were in the ranges of 82.9% ∼ 107.0% (spiked level 25 µg/kg), 74.1% ∼ 114.5% (spiked level 10 µg/kg) and 53.3% ∼ 123.7% (spiked level 2 µg/kg), respectively, and the relative standard deviations of all spiked levels were between 0.47% and 11.30%. The developed methodology was applied to the analysis of twenty sediment samples. A CZD of 2-methoxycarbazole (2-MOCZ) has been firstly detected in the sediments with the concentration up to1.4 µg/kg, indicating the environmental occurrence of CZDs and alerting to their potentially ecological risks in the environment.
咔唑衍生物（CZDs）是一类重要的含氮杂环化合物，已广泛应用于光电材料、染料、医药、超分子等领域。生产和产品使用过程中释放到环境中的咔唑衍生物的生态风险逐渐引起了人们的关注。然而，由于缺乏环境中咔唑衍生物的分析方法，进入环境的咔唑衍生物水平仍不清楚。在此，采用超高效液相色谱-高分辨率质谱（UHPLC-HRMS）结合QuEChERS预处理技术，建立了一种同时测定沉积物样品中13种与光电材料相关的咔唑衍生物的分析方法。对样品预处理和UHPLC-HRMS分析参数进行了优化。通过评估回收率、准确度、基质效应、方法检出限（LODs）等对所建立的方法进行了验证。仪器检测在1至1000μg/L的浓度范围内呈现线性响应，方法检出限为0.005至0.165μg/kg。大多数咔唑衍生物的平均回收率分别为加标水平25μg/kg时82.9%～107.0%、加标水平10μg/kg时74.1%～114.5%、加标水平2μg/kg时53.3%～123.7%，所有加标水平的相对标准偏差在0.47%至11.30%之间。所建立的方法应用于20个沉积物样品的分析。首次在沉积物中检测到浓度高达1.4μg/kg的2-甲氧基咔唑（2-MOCZ），表明咔唑衍生物在环境中的存在，并警示其在环境中潜在的生态风险。
