论文部分内容阅读
目的建立一种快速、高效、准确的同时测定环境水中12种致敏性分散染料的磁性碳纳米管-分散固相萃取-超快速液相色谱(d SPE-UFLC)方法。方法环境水采用氨基修饰磁性碳纳米管对12种致敏性分散染料进行-分散固相萃取技术富集,采用Shim-pack XR-ODSⅡ(75 mm×2.0 mm,2.2μm)和Shim-pack XR-ODSⅢ(75 mm×2.0 mm,2.2μm)双柱串联,以0.02 mol/L乙酸铵水溶液(内含0.08%甲酸)和乙腈(内含0.1%甲酸)为流动相,梯度洗脱,全波长(190 nm~700 nm)检测。结果 12种致敏性分散染料的浓度为1.00μg/L~500μg/L时,线性关系良好(r≥0.997 4),检出限为0.082μg/L~1.49μg/L,最低定量限为0.27μg/L~4.92μg/L,RSD为2.6%~8.2%;在低、中、高3种加标水平下,回收率分别为76.2%~100%、80.6%~98.4%、79.2%~98.9%。磁性碳纳米管的富集倍数为100倍。结论本法可用于环境水样中上述12种致敏性分散染料的快速测定。
OBJECTIVE To establish a rapid, efficient and accurate method for the simultaneous determination of 12 sensitized disperse dyes in environmental water by magnetic carbon nanotube-dispersive solid phase extraction-ultra fast liquid chromatography (d SPE-UFLC). Methods The aqueous ammonia modified magnetic carbon nanotubes were used to enrich 12 kinds of sensitized disperse dyes by dispersive solid-phase extraction. The Shim-pack XR-ODSⅡ (75 mm × 2.0 mm, 2.2 μm) and Shim-pack XR -ODSⅢ (75 mm × 2.0 mm, 2.2 μm) was used as the mobile phase in 0.02 mol / L ammonium acetate aqueous solution (containing 0.08% formic acid) and acetonitrile (190 nm ~ 700 nm) detection. Results The linear range of the 12 sensitizing disperse dyes was 1.00μg / L ~ 500μg / L (r ≥ 0.997 4). The limit of detection was 0.082μg / L ~ 1.49μg / L with the lowest limit of quantification being 0.27 μg / L ~ 4.92μg / L, RSD was 2.6% ~ 8.2%. The recoveries were 76.2% ~ 100%, 80.6% ~ 98.4%, 79.2% ~ 98.9 %. The enrichment factor of magnetic carbon nanotubes is 100 times. Conclusion This method can be used for the rapid determination of 12 allergenic disperse dyes in environmental water samples.