色谱2011,Vol.29Issue(1):87-90,4.DOI:10.3724/SP.J.1123.2011.00087
高效液相色谱-间接光度检测法测定己内酰胺酸团中的正己烷含量
Determination of hexane in the acid cluster of caprolactam by high performance liquid chromatography with indirect photometric detection
摘要
Abstract
An indirect photometric detection method for the determination of hexane in the acid cluster of caprolactam by high performance liquid chromatography was developed. Ultraviolet (UV) absorption background reagents were added in the mobile phase, and the hexane, nonabsorption in ultraviolet region, was directly determined by a UV detector. The effects of the mobile phase composition, species and concentration of the background reagents etc. on the analyzed results were studied. The optimization of the separation was performed on an Agilent HC-C18 column (250 mm ×4.6 mm, 5 μm). A solution of methanol-water (85∶15, v/v) containing 1.17 mmol/L 1,5-naphthalene disulfonic acid was used as mobile phase at a flow rate of 1.0 mL/min and the column temperature was set at 35 ℃. The gradient of wavelength was adopted to adjust the relative size of systematic peaks and the target peaks. The linear relationship in the range of 0.5 - 20 mg/kg with a correlation coefficient of 0.999 93 in this method was obtained. The recoveries and relative standard deviation for the hexane in the acid cluster of caprolactam were 98.45% - 102.3% and 2.53%, respectively. The detection limit was 0.03 mg/kg. The method is simple, and has good selectivity, high sensitivity and strong anti-interference ability for the accurate determination of hexane in practical samples quickly.关键词
高效液相色谱/间接光度检测/紫外检测/本底试剂/正己烷/己内酰胺酸团分类
化学化工引用本文复制引用
李立南,段正康,曾红艳,贺玉平,陈秋云..高效液相色谱-间接光度检测法测定己内酰胺酸团中的正己烷含量[J].色谱,2011,29(1):87-90,4.基金项目
湖南省科技厅项目(No. 2009FJ3043). (No. 2009FJ3043)