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    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

    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%.

       

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