In the present study, a novel and reliable analytical method was developed and validated for the simultaneous determination of 1,3,5-tris(2,3-dibromopropyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione (TDBP-TAZTO) and 2,4,6-tris(2,4,6-tribromophenoxy)-1,3,5-triazine (TTBP-TAZ) in environmental samples using high-performance liquid chromatography coupled to a tandem mass spectrometer. Firstly, for optimization of the liquid chromatography separation, mobile phases, oven temperatures, modifiers, and buffers were varied. Afterwards, the extraction efficiency of sediment and fish samples was tested with different techniques (pressurized liquid, solid-liquid, ultrasound-assisted, and Soxhlet extraction). Additionally, cleanup using modified multilayer silica gel (sediment) and gel permeation chromatography as well as Florisil® columns (fish) with several solvent mixtures were performed. The best results were obtained with the pressurized liquid extraction (optimal conditions: extraction solvent 100% toluene, extraction time 20 min, cycles two, extraction temperature 100 °C, and flushing volume 60%) compared to other solvent extraction methods. On the basis of this optimized analytical procedure, the method was validated with satisfactory values of correlation coefficient (R²) between 0.998 and 0.999 for both matrices in the calibration range of 2.0–502.0 μg kg⁻¹ for TDBP-TAZTO and 16.6–770.6 μg kg⁻¹ for TTBP-TAZ in sediment samples as well as 4.8–303.5 μg kg⁻¹ and 47.4–742.5 μg kg⁻¹ in fish samples (bream), respectively. Mean recoveries (n = 5) were calculated for both analytes with spiked matrices at one concentration level (100 μg kg⁻¹) between 98 and 114% with intra-day relative standard deviations less than 11%. The inter-day precision (n = 15) was also acceptable for both compounds < 11%. It was found that the limit of detection and limit of quantification were in the range of 0.4–1.3 μg kg⁻¹ for TDBP-TAZTO and 10–28 μg kg⁻¹ for TTBP-TAZ in surface sediment samples and 7–25 μg kg⁻¹ and 22–80 μg kg⁻¹ in fish samples (bream), respectively. The results indicated that these analytical methods could provide reliable and efficient approaches for quantification of TDBP-TAZTO and TTBP-TAZ in sediment and fish samples.

在本研究中，开发了一种新颖且可靠的分析方法，并验证了该方法可同时测定1,3,5-三（2,3-二溴丙基）-1,3,5-三嗪-2,4,6（1H）使用高性能液体的环境样品中的，3H，5H）-三酮（TDBP-TAZTO）和2,4,6-三（2,4,6-三溴苯氧基）-1,3,5-三嗪（TTBP-TAZ）色谱联用质谱仪。首先，为了优化液相色谱分离，改变了流动相，柱箱温度，改性剂和缓冲液。之后，使用不同的技术（加压液体，固液，超声辅助和索氏提取）测试了沉积物和鱼类样品的提取效率。另外，使用改良的多层硅胶（沉积物）和凝胶渗透色谱法以及带有几种溶剂混合物的Florisil®色谱柱（鱼）进行净化。与其他溶剂萃取方法相比，加压液体萃取（最佳条件：萃取溶剂100％甲苯，萃取时间20分钟，两次循环，萃取温度100°C和冲洗体积60％）获得了最佳结果。在此优化分析程序的基础上，该方法以令人满意的相关系数值进行了验证（[R ²）0.998〜0.999为2.0-502.0微克公斤的校准范围两个矩阵之间^-1为TDBP-TAZTO和16.6-770.6微克千克^-1为TTBP-TAZ沉积物样品中以及4.8-303.5微克公斤^-鱼样品（鲷）中分别为¹和47.4–742.5μgkg ^-1。 计算两种加标浓度为100 µg kg ^-1的分析物在98％至114％之间的平均回收率（n = 5），日内相对标准偏差小于11％。 对于两种<11％的化合物，日间精度（n = 15）也可以接受。发现检出限和定量限在0.4–1.3μgkg范围内^-1用于TDBP-TAZTO和10-28微克千克^-1为TTBP-TAZ表面沉积物样品和7-25微克千克^-1和22-80微克千克^-1鱼样品中（鲷），分别。结果表明，这些分析方法可为定量分析沉积物和鱼类样品中的TDBP-TAZTO和TTBP-TAZ提供可靠而有效的方法。