摘要
本文建立了淡水养殖水体中呋喃丹的全自动固相萃取-超高效液相色谱检测方法。选取HLB固相萃取小柱作为水样的富集和净化小柱,水样以5 mL·min^(-1)的速度上样,用10 mL甲醇洗脱。洗脱液经浓缩、定容后,采用超高效液相色谱-荧光检测法分析,色谱柱为ACQUITY UPLC BEH C_(18)柱(100 mm×2.1 mm,粒径1.7μm),流动相为乙腈-水(40∶60,V/V),流速为0.200 mL·min^(-1),激发波长为270 nm,发射波长为310 nm。呋喃丹在20~1 000μg·L^(-1)范围内线性关系良好,相关系数R^2>0.999,方法检出限为0.100μg·L^(-1),定量限为0.250μg·L^(-1),在0.250、2.50、10.0μg·L^(-1)三种加标浓度水平下,平均加标回收率为90.4%~96.3%,相对标准偏差为2.55%~5.10%。该方法自动化程度高、操作简便、快速准确、稳定性好,适用于淡水养殖水体中呋喃丹的测定。
A new method was developed for the determination of carbofuran in freshwater aquaculture water by ultra high pressure liquid chromatography（ UPLC） combined with automatic solid phase extraction（ SPE）.The water sample flowed through HLB SPE cartridge with a flow rate of 5 mL·min^-1,and the analyte was eluted with 10 mL methanol in SPE cartridge. After concentrating and redissolving with acetonitrile-water（ 40∶ 60,V/V）,the eluent was analyzed by ultra high performance liquid chromatography with fluorescence detection. The analysis conditions were as the follows： chromatographic column was ACQUITY UPLC BEH C_（18）（ 100 mm × 2. 1 mm,1. 7 μm）,mobile phase was acetonitrile-water（ 40∶ 60,V/V）,flow rate was 0. 200 mL·min^-1,excitation wavelength was 270 nm,emission wavelength was 310 nm. The correlation coefficients of carbofuran standard curve was more than 0. 999 in the range of 20 ~ 1 000 μg·L^-1. The limit of detection was 0. 100 μg· L^-1 and the limit of quantitation was 0. 250 μg · L^-1. The average recoveries were in the range of 90. 4% ~ 96. 3% and the relative standard deviations were 2. 55% ~ 5. 10% at 0. 250 μg·L^-1,2. 50 μg·L^-1 and 10. 0 μg·L^-1 spiked levels. The method was highly automated,simple,rapid,accurate and stable,and also suitable for the determination of carbofuran in freshwater aquaculture water.
出处
《渔业研究》
2017年第5期386-391,共6页
Journal of Fisheries Research
基金
福建省科技计划社会发展引导性(重点)项目(2016Y0004)
关键词
呋喃丹
超高效液相色谱
全自动固相萃取
淡水养殖水体
carbofuran
ultra high performance liquid chromatography
automatic solid phase extraction
fresiiwater aquaculture water
