分散固相萃取-超快速液相色谱-二极管阵列法同时测定环境水中12种致敏性分散染料

Simultaneous detection of 12 allergenic disperse dyes in environmental water by dispersive soild phase extraction coupled with ultra fast liquid hromatography-diode array detection

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 develop a rapid,effective and accurate method for the simultaneous determination of 12 allergenic disperse dyes in environmental water sample by carbon nano-tube-dispersive soild phase extraction-ultra fast liquid chromatography-diode array detection（ CNTs-d SPE-UFLC-DAD）. Methods The 12 allergenic disperse dyes in the environment water were enriched by amino-functionalized magnetic CNTs-dispersive solid phase extraction. Chromatographic separation was performed on 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） columns. With 0. 02 mol / L ammonium acetate solution（ containing 0. 08% formic acid） and acetonitrile（ containing0. 1% formic acid） as mobile phases for gradient elution,the 12 allergenic disperse dyes were detected at full wavelength（ 190 nm-700 nm）. Results Good linearity was obtained when the concentration of 12 allergenic disperse dyes was within1. 00 μg / L-500 μg / L,with the determination coefficients（ r ≥ 0. 997 4）. The limits of detection（ LODs） were within0. 082 μg / L-1. 49 μg / L,and the limits of quantification（ LOQs） were within 0. 27 μg / L-4. 92 μg / L. The relative standard deviations（ RSDs） were within 2. 6%-8. 2%. Recoveries were within 76. 2%-100%,80. 6%-98. 4% and 79. 2%-98. 9% at the low,medium and high spiked levels,respectively. And the enrichment times of magnetic carbon nanotubes was100. Conclusion The developed method can be applied to the routine analyses for the determination of 12 allergenic disperse dyes in environmental water samples.