分析化学2012，Vol.40Issue(4)：545-550,6.DOI:10.3724/SP.J.1096.2012.10895
固相萃取-高效液相色谱-质谱法测定污水中糖皮质激素
Determination of Glucocorticoids in Wastewater by Orthogonal Test Solid Phase Extraction-High Performance Liquid Chromatography-Mass Spectrometer
摘要
Abstract
A comprehensive analytical method based on solid-phase extraction (SPE) and ultra performance liquid chromatography-electrospray tandem mass spectrometry (UPLC-MS/MS) has been developed for the simultaneous determination of seven glucocorticoids in wastwater sample. Several single factor experiments were applied to analyze the effect of the solvent and volume used for elution, Ph adjustment of the water sample, and the wash solution on SPE. Based on the single factor tests, the L9(34) orthogonal test was used to further optimize extraction parameters. The primary and secondary factors were distinguished by visual analysis and analysis of variance. The optimum extraction process was as follows: eluting solvent was ethyl acetate, elution volume was 10mL, the Ph value was 5.0 and washing solvent was 20% (V/V) methanol in HPLC grade water. The correlation coefficient (r2) of the calibration curve was over 0. 9976, in linear range of 1 - 100 μg/L. The limits of detection (LOD) were between 1. 56 and 10. 59 ng/L. The recoveries at the spiked level of 20 - 100 ng/L were 72. 48% to 101. 42%, with the relative standard deviation (RSD) less than 10.9%.关键词
固相萃取/超高效液相色谱-串联质谱法/糖皮质激素/正交实验Key words
Solid phase extration/Ultra performance liquid chromatography-tandem mass spectrome-try/Glucocorticoid/Orthogonal test引用本文复制引用
谭丽超,葛峰,单正军,王懿..固相萃取-高效液相色谱-质谱法测定污水中糖皮质激素[J].分析化学,2012,40(4):545-550,6.基金项目
本文系环境保护部公益性项目(No.200809094)资助 （No.200809094）
