摘要
建立了一种快速、高效、灵敏的基质分散-磁性固相萃取/液相色谱（d MSPE-HPLC）方法,用于海水中5种氯酚类（CPs）污染物残留量的测定。样品用五氯酚分子印迹氨基功能化磁性复合材料富集,在C8反相液相色谱柱（250 mm×4.6 mm×5.0μm）上分离,以甲醇-5 mmol/L乙酸铵水溶液（体积比70∶30）为流动相,230 nm处检测。考察了样品p H值、萃取时间和洗脱剂的种类与用量对CPs富集回收率的影响。结果表明,在最佳实验条件下,5种CPs在1~5 000 ng/L浓度范围内呈良好的线性关系,相关系数（r2）均大于0.998 9;平均回收率为86.5%~98.8%,相对标准偏差（RSDs）为0.8%~8.6%;检出限（LODs）为0.18~1.20 ng/L,定量下限（LOQs）为0.6~4.0 ng/L。方法可用于海水中CPs类化合物的快速筛查和确证分析。
A rapid,sensitive and accurate method for the simultaneous determination of 5 kinds of chlorophenols（ CPs） in seawater samples by dispersive magnetic solid phase extraction- liquid chromatography（ d MSPE- HPLC） was developed. The seawater samples were firstly enriched with pentachlorophenol-imprinted amino-functionalized nano-Fe3O4-polymer magnetic composite material（ n Fe3O4@ MIPNH2- polymer）,then separated on a C8 analytic column（ 250 mm × 4. 6 mm × 5. 0μm） using methanol- NH4 Ac solution（ 70 ∶ 30） as mobile phase and detected at 230 nm via UV detector. The results showed that under the optimal condition,the calibration curves were linear in the range of 1- 5 000 ng / L with correlation coefficients（ r2） higher than 0. 998 9 for target chlorophenols. The spiked recoveries were between 86. 5% and 98. 8% with relative standard deviations（ RSDs） of 0. 8%- 8. 6%. The limits of detection（ LODs） were in the range of 0. 18- 1. 20 ng / L and the limits of quantitation（ LOQs） were between 0. 6 ng / L and 4. 0 ng / L. The developed method could be applied in the routine analysis of chlorophenols in seawater samples.
出处
《分析测试学报》
CAS
CSCD
北大核心
2015年第11期1213-1219,共7页
Journal of Instrumental Analysis
基金
浙江省自然科学基金(LY14B04003)
宁波市自然科学基金(2014A610092)
国家级大学生创新创业训练计划项目(2014)
浙江省新苗计划项目(2014)
关键词
氨基功能化
分子印迹磁性材料
氯酚类污染物
海水
基质分散-磁性固相萃取
amino-functionalized
molecular-imprinted magnetic material
chlorophenols
seawater
dispersive solid phase extraction（d MSPE）
