固相萃取-高效液相色谱/荧光法测定全血中苯胺

Determination of aniline in whole blood by using solid-phase extraction and high performance liquid chromatography with fluorescence detector

目的建立全血中痕量苯胺的固相萃取-高效液相色谱荧光检测方法。方法样品用水稀释,乙腈提取后,用Cleanert NH2固相萃取小柱进行净化,在Kromasil C18柱（250 mm×4.6 mm i.d.,5μm）上以水/乙腈（20/80,V/V）为流动相进行等度洗脱,荧光检测波长λex为225 nm,λem为335 nm,外标法定量。结果苯胺在3.0-200.0μg/L范围内具有良好的线性,相关系数0.9992,定量限为3.0μg/L,回收率为87.5%-104.4%,日内RSDs为3.1%-6.6%,日间RSDs为6.4%-8.6%。结论该方法简便、快速、干扰少、特异性强,适用于全血中痕量苯胺的检测。

Objective To establish a method for the determination of trace aniline in whole blood by using solid-phase extraction and high performance liquid chromatography with fluorescence detector. Methods After the whole blood was diluted by water,extracted by acetonitrile,cleaned and enriched by Cleanert NH2solid-phase extraction（ SPE） cartridge,separation was performed on a Kromasil C18column（ 250 mm × 4. 6 mm i. d.,5 μm） with the mobile phase of water / acetonitrile（ 20 /80,V / V）. Detection was carried out by fluorescence detector at λex225 nm and λem335 nm. Results Calibration curve was linear in the range of 3. 0- 200. 0 μg / L with a correlation coefficient of0. 9992,and the limit of quantitation（ LOQ） was 3. 0 μg / L. The extraction recoveries were87. 5%- 104. 4%,and the intra-day and inter-day RSDs were 3. 1%- 6. 6% and 6. 4%- 8. 6%, respectively. Conclusion The developed method is simple, fast, little interference,good specificity for the satisfactory determination of trace aniline in whole blood.