De Toffoli Ana L, Fumes Bruno H, Lanças Fernando M
a University of Sao Paulo, Institute of Chemistry at Sao Carlos , Department of Chemistry , São Carlos , SP , Brazil.
J Environ Sci Health B. 2018;53(7):434-440. doi: 10.1080/03601234.2018.1438831. Epub 2018 Feb 22.
On-line in-tube solid phase microextraction (in-tube SPME) coupled to high performance liquid chromatography and tandem mass spectrometry (HPLC-MS/MS) was successfully applied to the determination of selected triazines in water samples. The method based on the employment of a packed column containing graphene oxide (GO) supported on aminopropyl silica (Si) showed that the extraction phase has a high potential for triazines extraction aiming to its physical-chemical properties including ultrahigh specific surface area, good mechanical and thermal stability and high fracture strength. Injection volume and loading time were both investigated and optimized. The method validation using Si-GO to extract and concentrate the analytes showed satisfactory results, good sensitivity, good linearity (0.2-4.0 µg L) and low detection limits (1.1-2.9 ng L). The high extraction efficiency was determined with enrichment factors ranging from 1.2-2.9 for the lowest level, 1.3-4.9 intermediate level and 1.2-3.0 highest level (n = 3). Although the analytes were not detected in the real samples evaluated, the method has demonstrated to be efficient through its application in the analysis of spiked triazines in ground and mineral water samples.
在线管内固相微萃取(管内固相微萃取)与高效液相色谱和串联质谱联用(HPLC-MS/MS)成功应用于水样中选定三嗪类化合物的测定。该方法采用填充有负载在氨丙基硅胶(Si)上的氧化石墨烯(GO)的柱子,结果表明,基于其超高比表面积、良好的机械和热稳定性以及高断裂强度等物理化学性质,该萃取相在三嗪类化合物萃取方面具有很大潜力。对进样体积和加载时间进行了研究和优化。使用Si-GO萃取和浓缩分析物的方法验证显示出令人满意的结果,具有良好的灵敏度、良好的线性(0.2 - 4.0 μg/L)和低检测限(1.1 - 2.9 ng/L)。测定的高萃取效率表现为,最低水平的富集因子为1.2 - 2.9,中间水平为1.3 - 4.9,最高水平为1.2 - 3.0(n = 3)。尽管在所评估的实际样品中未检测到分析物,但该方法通过应用于加标三嗪类化合物的地下水和矿泉水样品分析已证明是有效的。