固相萃取-高效液相色谱-串联质谱法同时测定养殖海水中23种抗生素

Simultaneous determination of 23 antibiotics in mariculture water using solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry

建立了固相萃取？高效液相色谱？串联质谱（ SPE？HPLC？MS／MS）同时检测水中6类23种抗生素的分析方法。水样用固相萃取柱富集净化，通过对比水样在不同上样pH、洗脱液用量等条件下的回收率，优化了前处理方法。采用0.1％（v／v）甲酸-1 g／L甲酸铵水溶液和甲醇？乙腈（1∶1， v／v）体系作为流动相，经过梯度洗脱进行分离，在HPLC-MS／MS多反应监测模式下进行定性定量分析。结果显示，23种抗生素的方法检出限（ MDL）范围为0.1～2.9 ng／L，加标回收率为47.3％～132.6％。采用该方法对东营海水养殖区5个养殖池水样进行了检测，除青霉素类之外的各类抗生素均有检出，其中磺胺增效剂甲氧苄氨嘧啶的检出率达100％，氯霉素类抗生素氟甲砜霉素检出的最高质量浓度达到261.0 ng／L。结果表明，所建立的方法高效、灵敏、可靠，可用于海水中多种抗生素的分析。

A method for the determination of 23 developed by using solid-phase extraction and high antibiotics from 6 categories in water was performance liquid chronlatography-tandem mass spect：rometry （SPE-HPLC-MS/MS）. Water samples were enriched and cleaned-up by sol- id-phase extraction cart, ridges. The MS detection parameters of the analyzed antibiotics, the pH values of loading buffers and the volumes of the eluents were optimized by comparing the sam- pie recoveries under different conditions. All antibiotics were separated by gradient elution with the mobile phases of 0. 1% （v/v） formic acid and I g/L ammonium formate in water and aceto- nitrile-methanol （ 1：1, v/v） mixture. The eluate was then analyzed by IIPLC-MS/MS in both positive and negative electrospray ionization conditions with mult：iple reaction monitoring （MRM） mode. The method detection limits （MDLs） were in the range of 0. 1-2.9 ng/L and the recoveries of 23 antibiotics in water ranged from 47, 3% to 132.6%. The developed method was applied to the analysis of 5 water samples from mariculture ponds located in Dongying City, Shandong Province. The results showed that the antibiotics could be detected in all water sam- ples. The trimethoprim showed the highest detection rate, and the florfenicol had the highest mass concentration which reached 261.0 ng/L. The results showed that the developed method is efficient, sensitive and reliable, which is suitable for the detection of antibiotics in seawater samples.