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建立了一种利用高效液相色谱-质谱联用技术快速筛查检测水体中13种β-内酰胺类药物残留的方法。水样经高速离心后过0.22μm微孔滤膜直接进样,以0.05%甲酸水溶液和甲醇-乙腈(4∶6,v/v)混合溶液为流动相进行梯度洗脱,经Atlantis dC-C18柱(150 mm×4.6 mm,5μm,Waters公司)分离,采用电喷雾离子源正离子电离、多反应监测模式检测。13种β-内酰胺类化合物在线性范围内的线性关系均良好,相关系数( r2)均大于0.99,回收率均在81.4%~102.3%范围内,相对标准偏差均小于11%( n=7),检出限均在1.5~10 ng/L范围内。该方法快速、简便、灵敏,重现性好,为开展水体中抗生素污染水平的调查与监测提供了技术支持。

A rapid method for the simultaneous screening and determination of 13 β-lactam res-idues in water was developed by high performance liquid chromatography-tandem mass spec-trometry( HPLC-MS/MS). After high speed centrifugation,the sample was filtered through a 0. 22 μm microporous filter membrane,and then separated on an Atlantis dC-C 18 column( 150 mm×4. 6 mm,5 μm,Waters)with the gradient elution of water(containing 0. 05%(v/v)for-mic acid)and methanol-acetonitrile(4∶6,v/v). The electrospray ionization(ESI)source in positive ion mode was used for multiple reaction monitoring( MRM)mode. The 13 β-lactam chemical components showed good linear relationships in their concentration ranges with the correlation coefficients( r2 )more than 0. 99. The recoveries were all in the range of 81. 4%-102. 3%,and the relative standard deviations( RSDs)were all less than 11%( n=7). The limits of detection( LODs)were in the range of 1. 5-10 ng/L. This method is rapid,simple,sensi-tive,accurate,and provides the basis for the investigation and monitoring of the pollution lev-els of the antibiotics in water.

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