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    固相萃取-液相色谱-串联质谱法测定猪栏废水中10种抗生素

    LC-MS/MS Determination of 10 Antibiotics in Swinery Waste Water with Solid Phase Extraction

    • 摘要: 应用固相萃取-液相色谱-串联质谱法测定养猪废水中10种抗生素的含量。水样由盐酸调节pH至2.5~4.0,流经Oasis HLB固相萃取柱富集后再用甲醇洗脱。以Aglient eclipse XDB C18色谱柱为分离柱,以不同体积比的0.1%(体积分数)甲酸溶液和乙腈混合液为流动相进行梯度洗脱,采用电喷雾正离子源多反应监测模式检测。10种抗生素在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.03~3.5 μg·L-1之间。加标回收率在53.2%~104%之间,测定值的相对标准偏差(n=6)在0.5%~6.3%之间。

       

      Abstract: LC-MS/MS was applied to the determination of 10 antibiotics in swinery waste water with solid phase extraction. The water sample was acidified to pH 2.5 to 4.0 with HCl, and enriched by passing through Oasis HLB SPE column. The column was eluted with methanol. For LC separation, aglient eclipse XDB C18 column was used as stationary phase, and the mixture of 0.1% (φ) formic acid solution and acetonitrile mixed in different ratio was used as mobile phase in gradient elution. ESI+ and multi-reaction monitoring were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 10 antibiotics were kept in definite ranges. Detection limits (3S/N) found were ranged from 0.03 to 3.5 μg·L-1. Values of recovery found by standard addition method were in the range of 53.2%-104%, with values of RSD′s (n=6) in the range of 0.5%-6.3%.

       

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