色谱2018，Vol.36Issue(4)：370-375,6.DOI:10.3724/SP.J.1123.2017.11018
基于整体柱的固相萃取-高效液相色谱法测定尿液中4种羟基多环芳烃
Determination of four hydroxyl polycyclic aromatic hydrocarbons in urine by solid-phase extraction with monolithic column coupled with high performance liquid chromatography
摘要
Abstract
A method based on monolithic column solid-phase extraction(SPE)coupled with high performance liquid chromatography(HPLC)was developed for the simultaneous determination of four hydroxyl polycyclic aromatic hydrocarbons(OH-PAHs)in urine. A poly (butyl methacrylate-co-ethylene dimethacrylate)monolithic column was prepared in a syringe and was used as the sorbent. The parameters influencing SPE,such as loading volume,wash-ing solvent,eluent,and elution volume,were investigated in detail. Under the optimized condi-tions,the linearities were obtained in range of 1.2-200.0 ng/mL,and the LODs and LOQs of the analytes were 0.06-0.09 ng/mL and 0.20-0.30 ng/mL,respectively. The intra-day and inter-day relative standard deviations were 1.4% -5.3% and 2.6% -7.3%,respectively. The recoveries evaluated using the spiked(3 ng/mL)urine samples of coke oven workers ranged from 78.2% to 117.0%. The feasibility of the developed method was further demonstrated for the analysis of the real samples. The results indicated that the reusable monolithic column enabled effective purification and enrichment of the four OH-PAHs in urine,and can be applied to the analysis of OH-PAHs in urine due to its simplicity and accuracy.关键词
高效液相色谱/固相萃取/聚合物整体柱/羟基多环芳烃/尿液Key words
high performance liquid chromatography(HPLC)/solid-phase extraction(SPE)/polymer monolithic column/hydroxyl polycyclic aromatic hydrocarbons(OH-PAHs)/urine分类
化学化工引用本文复制引用
胡桂羽,王曼曼,念琪循,李娜,董鑫鑫,郝玉兰,王茜,王学生..基于整体柱的固相萃取-高效液相色谱法测定尿液中4种羟基多环芳烃[J].色谱,2018,36(4):370-375,6.基金项目
国家自然科学基金(21305028) （21305028）
河北省自然科学基金(H2017209232,H2016209018) （H2017209232,H2016209018）
华北理工大学培育基金项目(JQ201717).National Natural Science Foundation of China(No.21305028) （JQ201717）
Natural Science Foundation of Hebei Prov-ince(Nos.H2017209232,H2016209018) （Nos.H2017209232,H2016209018）
Training Foundation of North China University of Science and Technology(No.JQ201717). （No.JQ201717）
