色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2015年
5期
449-454
,共6页
孙红%娄大伟%连丽丽%韩雪%郭亭秀%陈慧君
孫紅%婁大偉%連麗麗%韓雪%郭亭秀%陳慧君
손홍%루대위%련려려%한설%곽정수%진혜군
磁性固相萃取%高效液相色谱%微囊藻毒素%水%磁性纳米粒子%介孔
磁性固相萃取%高效液相色譜%微囊藻毒素%水%磁性納米粒子%介孔
자성고상췌취%고효액상색보%미낭조독소%수%자성납미입자%개공
magnetic solid-phase extraction(MSPE)%high performance liquid chromatogra-phy( HPLC)%microcystins(MCs)%water%magnetic nanoparticles%mesoporous
通过水热合成和常温合成的方法制备了介孔 Fe3O4@mSiO2@Cu2+磁性复合纳米粒子(NPs),其具有均匀的尺寸大小、良好的磁性能和特异的选择性。本研究将合成的 NPs 用作磁性固相萃取( MSPE)介质,结合高效液相色谱( HPLC)发展了一种测定水样品中痕量微囊藻毒素 MC-LR的方法。在优化 MSPE和 HPLC条件后,该方法在0.1~15μg/L范围内呈现良好的线性,线性相关系数( r)为0.9994,检出限为0.025μg/L,定量限为0.082μg/L。进一步将该方法用于水样中痕量藻毒素分析,结果发现回收率达到78%。这一结果表明:制得的磁性纳米粒子具有良好的萃取性能,可有效用于水样中痕量藻毒素的测定。
通過水熱閤成和常溫閤成的方法製備瞭介孔 Fe3O4@mSiO2@Cu2+磁性複閤納米粒子(NPs),其具有均勻的呎吋大小、良好的磁性能和特異的選擇性。本研究將閤成的 NPs 用作磁性固相萃取( MSPE)介質,結閤高效液相色譜( HPLC)髮展瞭一種測定水樣品中痕量微囊藻毒素 MC-LR的方法。在優化 MSPE和 HPLC條件後,該方法在0.1~15μg/L範圍內呈現良好的線性,線性相關繫數( r)為0.9994,檢齣限為0.025μg/L,定量限為0.082μg/L。進一步將該方法用于水樣中痕量藻毒素分析,結果髮現迴收率達到78%。這一結果錶明:製得的磁性納米粒子具有良好的萃取性能,可有效用于水樣中痕量藻毒素的測定。
통과수열합성화상온합성적방법제비료개공 Fe3O4@mSiO2@Cu2+자성복합납미입자(NPs),기구유균균적척촌대소、량호적자성능화특이적선택성。본연구장합성적 NPs 용작자성고상췌취( MSPE)개질,결합고효액상색보( HPLC)발전료일충측정수양품중흔량미낭조독소 MC-LR적방법。재우화 MSPE화 HPLC조건후,해방법재0.1~15μg/L범위내정현량호적선성,선성상관계수( r)위0.9994,검출한위0.025μg/L,정량한위0.082μg/L。진일보장해방법용우수양중흔량조독소분석,결과발현회수솔체도78%。저일결과표명:제득적자성납미입자구유량호적췌취성능,가유효용우수양중흔량조독소적측정。
Mesoporous magnetic nanoparticles of Fe3O4@mSiO2@Cu2+ were synthesized by two methods of hydrothermal synthesis and room temperature synthesis. The synthesized meso-porous Fe3O4@mSiO2@Cu2+ nanoparticles presented uniform sizes,good magnetic properties and specific selectivity. In this work,a novel magnetic solid-phase extraction( MSPE)method based on mesoporous Fe3O4@mSiO2@Cu2+ nanoparticles( NPs)coupled with high perform-ance liquid chromatography( HPLC ) was developed for the simultaneous extraction of trace amount of microcystin-LR( MC-LR ) in water samples. The MSPE extraction conditions and HPLC conditions were optimized. The results showed that good linear relationship( r=0. 999 4) was obtained between peak area and mass concentration of MC-LR in the range of 0. 1-15μg/L. The limit of detection was 0. 025 μg/L,and the limit of quantification was 0. 082 μg/L. Furthermore,this method was used for the analysis of algal toxins in water samples with the recovery of 78%. The results indicated that Fe3O4@mSiO2@Cu2+ magnetic nanoparticles were good pretreatment alternatives for the concentration of microcystin-LR in water samples.