全自动在线SPE-UPLC-MS/MS测定中水中15种喹诺酮

reclaimed water; quinolones; online solid phase extraction; super high performance font-size: 10pt; ">liquid chromatography-tandem mass spectrometry

建立了中水中15种喹诺酮类物质的全自动在线固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)测定方法。在中水样品加入0.2%甲酸酸化后加入5%甲醇，进样量为5 mL，仪器自动完成6个步骤：加载样品、淋洗、洗脱、SPE柱的再生、被测物的分离和质谱分析测定。分析方法采用电喷雾正离子扫描（ESI⁺），多反应监测（MRM）模式检测，外标法定量。 在加标浓度范围为0.05~5 μg/L时， 15种喹诺酮标准曲线线性良好，相关系数（R²）均大于0.991，回收率范围为84.4%~116.2%（n=6），RSD≤19.92%，检出限（LOD）范围为0.7~8.7 ng/L。采用该方法检测了30个实际中水样品，其中13个中水样品检出了7种喹诺酮，浓度范围为0.004 2~0.47 μg/L。

A fully automated online solid phase extraction-super high performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS)method was developed for detecting 15 quinolones in reclaimed water samples. The samples were acidized with 0.2%formic acid, then added 5% methanol. The injection volume was 5 mL, and the instrument automatically completed 6 steps: loading sample, cleanup, elution, online SPE column regeneration, separation of the object and determination by mass spectrometry. The analytical methods were electrospray positive ion scanning (ESI ⁺), multi-reaction monitoring (MRM) mode detection, and external standard legal quantity. When the standard concentration range was 0.05-5 μg/L, the standard curve of 15 quinolones was linear and the correlation coefficient (R²) was greater than 0.991. The recovery range was 84.4%-116.2%(n=6), the RSD was no more than 19.92%, and the limit of detection (LOD) range was 0.7-8.7 ng/L. 30 reclaimed water samples were analyzed by this method. As a result, 7 quinolones were detected in 13 reclaimed water samples. The concentration of the compounds ranged from 0.004 2 to 0.47 μg/L.