色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
8期
897-903
,共7页
李爱梅%黄茁%卢文平%徐中其
李愛梅%黃茁%盧文平%徐中其
리애매%황촬%로문평%서중기
毛细管电泳%场放大电动进样%四环素%环境水体%基质效应
毛細管電泳%場放大電動進樣%四環素%環境水體%基質效應
모세관전영%장방대전동진양%사배소%배경수체%기질효응
capillary electrophoresis(CE)%field-amplified sample injection( FASI)%tetracy-clines(TCs)%environmental water%matrix effect
比较了毛细管电泳(CE)和高效液相色谱(HPLC)技术对水体中4种四环素类抗生素(四环素、土霉素、金霉素及强力霉素)的分离效果。实验考察了水体的基质效应( pH 值和水硬度)对分离的影响,优化了电泳条件,在压力进样模式(HDI)下,9.0 min 内4种抗生素可达到基线分离,与 HPLC 相比,CE 可以节省一半左右的分析时间。该方法具有良好的线性关系,检出限(LOD)在0.28~0.62 mg / L 之间,迁移时间和峰面积的相对标准偏差( RSD)(n =6)分别为0.42%~0.56%及2.24%~2.95%;自来水和鱼塘水中加标回收率分别在96.3%~107.2%之间和87.1%~105.2%之间。此外,利用场放大电动进样(FASI)对目标物进行柱内预浓缩,检测灵敏度较 HDI 进样模式提高,LOD 降至17.8~35.5μg / L,迁移时间和峰面积的 RSD( n =6)分别为0.85%~0.95%及1.69%~3.43%。CE具有样品前处理简单、分析速度快的特点,对环境水体中抗生素的检测具有明显的优势。
比較瞭毛細管電泳(CE)和高效液相色譜(HPLC)技術對水體中4種四環素類抗生素(四環素、土黴素、金黴素及彊力黴素)的分離效果。實驗攷察瞭水體的基質效應( pH 值和水硬度)對分離的影響,優化瞭電泳條件,在壓力進樣模式(HDI)下,9.0 min 內4種抗生素可達到基線分離,與 HPLC 相比,CE 可以節省一半左右的分析時間。該方法具有良好的線性關繫,檢齣限(LOD)在0.28~0.62 mg / L 之間,遷移時間和峰麵積的相對標準偏差( RSD)(n =6)分彆為0.42%~0.56%及2.24%~2.95%;自來水和魚塘水中加標迴收率分彆在96.3%~107.2%之間和87.1%~105.2%之間。此外,利用場放大電動進樣(FASI)對目標物進行柱內預濃縮,檢測靈敏度較 HDI 進樣模式提高,LOD 降至17.8~35.5μg / L,遷移時間和峰麵積的 RSD( n =6)分彆為0.85%~0.95%及1.69%~3.43%。CE具有樣品前處理簡單、分析速度快的特點,對環境水體中抗生素的檢測具有明顯的優勢。
비교료모세관전영(CE)화고효액상색보(HPLC)기술대수체중4충사배소류항생소(사배소、토매소、금매소급강력매소)적분리효과。실험고찰료수체적기질효응( pH 치화수경도)대분리적영향,우화료전영조건,재압력진양모식(HDI)하,9.0 min 내4충항생소가체도기선분리,여 HPLC 상비,CE 가이절성일반좌우적분석시간。해방법구유량호적선성관계,검출한(LOD)재0.28~0.62 mg / L 지간,천이시간화봉면적적상대표준편차( RSD)(n =6)분별위0.42%~0.56%급2.24%~2.95%;자래수화어당수중가표회수솔분별재96.3%~107.2%지간화87.1%~105.2%지간。차외,이용장방대전동진양(FASI)대목표물진행주내예농축,검측령민도교 HDI 진양모식제고,LOD 강지17.8~35.5μg / L,천이시간화봉면적적 RSD( n =6)분별위0.85%~0.95%급1.69%~3.43%。CE구유양품전처리간단、분석속도쾌적특점,대배경수체중항생소적검측구유명현적우세。
The system abilities of two chromatographic techniques,capillary electrophoresis (CE)and high performance liquid chromatography(HPLC),were compared for the analysis of four tetracyclines(tetracycline,chlorotetracycline,oxytetracycline and doxycycline). The pH, concentration of background electrolyte(BGE)were optimized for the analysis of the standard mixture sample,meanwhile,the effects of separation voltage and water matrix( pH value and hardness)effects were investigated. In hydrodynamic injection( HDI)mode,a good quantita-tive linearity and baseline separation within 9. 0 min were obtained for the four tetracyclines at the optimal conditions;the analytical time was about half of that of HPLC. The limits of detec-tion(LODs)were in the range of 0. 28-0. 62 mg / L,and the relative standard deviations(RSDs) (n = 6)of migration time and peak area were 0. 42% - 0. 56% and 2. 24% - 2. 95% ,respectively. The obtained recoveries spiked in tap water and fishpond water were at the ranges of 96. 3% -107. 2% and 87. 1% - 105. 2% ,respectively. In addition,the stacking method,field-amplified sample injection(FASI),was employed to improve the sensitivity,and the LOD was down to the range of 17.8-35.5 μg / L. With FASI stacking,the RSDs(n = 6)of migration time and peak area were 0. 85% -0. 95% and 1. 69% -3. 43% ,respectively. Due to the advantages of simple sam-ple pretreatment and fast speed,CE is promising in the analysis of the antibiotics in environ-mental water.