UHPLC Determination of 4 Nitrofurans in Water with Solid Phase Extraction
摘 要
采用固相萃取-超高效液相色谱法测定水体中呋喃西林、呋喃它酮、呋喃妥因、呋喃唑酮等4种硝基呋喃类药物的含量。样品经HLB固相萃取柱净化后,用氨水-甲醇(5+95)溶液洗脱。以BEH C18色谱柱为分离柱,以乙腈和含有0.1%(体积分数)甲酸的2 mmol·L-1乙酸铵溶液以体积比23比77组成的混合液为流动相,在检测波长360 nm处进行测定。4种硝基呋喃类药物的质量浓度均在5.0~200 μg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)为0.02 μg·L-1。以空白样品为基体进行加标回收试验,所得回收率在84.5%~97.2%之间,测定值的相对标准偏差(n=6)在1.5%~4.5%之间。
Abstract
UHPLC was applied to the determination of 4 nitrofurans, i.e. furacilin, furaltadone, nitrofurantoin and furazolidone in water with solid phase extraction. The sample was purified by passing through HLB solid phase extraction column and eluted with a mixture of ammonia and methanol (5+95). BEH C18 chromatographic column was used as stationary phase, and a mixture of acetonitile and 2 mmol·L-1 ammonium acetate solution (containing 0.1% formic acid) (23+77) was used as mobile phase. UV-detection at 360 nm was adopted in the determination. Linear relationships between values of peak area and mass concentration of the 4 nitrofurans were kept in the same range of 5.0-200 μg·L-1, with detection limit (3S/N) of 0.02 μg·L-1.On the base of blank sample, test for recovery was made by standard addition method;values of recovery found were in the range of 84.5%-97.2%, with RSD′s (n=6) in the range of 1.5%-4.5%.
中图分类号 O652.63
所属栏目 工作简报
基金项目 浙江省自然科学基金项目(LQ13C200004);浙江省科技计划项目(2012F20026
收稿日期 2014/3/19
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备注严忠雍(1990-),男,浙江温州人,助理工程师,研究方向为渔业环境监测和水产品质量安全。
引用该论文: YAN Zhong-yong,ZHANG Xiao-jun,LI Pei-pei,YU Liang,LONG Ju,ZHU Yin,WANG Jian. UHPLC Determination of 4 Nitrofurans in Water with Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(11): 1369~1372
严忠雍,张小军,李佩佩,喻亮,龙举,祝银,王建. 固相萃取-超高效液相色谱法测定水体中4种硝基呋喃类药物[J]. 理化检验-化学分册, 2014, 50(11): 1369~1372
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【6】王蕾,鲍恩东.饲料中硝基呋喃类药物高效液相色谱检测方法的建立[J].中国农业大学学报, 2011,16(2):125-132.
【7】魏晋梅,周围,毕阳,等.饲料中三种硝基呋喃类药物的超高效液相色谱同步检测方法[J].饲料工业, 2007(10):48-50.
【8】CHU P-S, LOPEZ M I. Determination of nitrofuran residues in milk of dairy cows using liquid chromatography-tandem mass spectrometry[J]. Journal of Agricultural and Food Chemistry, 2007,55(6):2129-2135.
【9】林黎明,林回春,刘心同,等.固相萃取高效液相色谱-质谱法测定动物组织中硝基呋喃代谢产物[J].分析化学, 2005,33(5):707-710.
【10】孙良娟,李红权,梁锋,等.高效液相色谱串联质谱法同时测定饲料中4种硝基呋喃类抗生素[J].分析测试学报, 2013,32(8):978-982.
【11】张静,彭新然,王向军,等.高效液相色谱-串联质谱法测定香肠中硝基呋喃代谢物[J].理化检验-化学分册, 2007,43(10):858-860.
【12】李佐卿,俞雪钧,倪梅林,等.高效液相色谱-串联质谱法测定水产品中硝基呋喃代谢物[J].理化检验-化学分册, 2008,44(11):1028-1030.
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