On-line coupling of solid-phase extraction to liquid chromatography-tandem mass spectrometry for the determination of macrolide antibiotics in environmental water |
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Authors: | Jie Ding Nanqi Ren Lan Ding |
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Affiliation: | a State Key Laboratory of Urban Water Resource and Environment, Harbin Institute of Technology, 202 Haihe Road, Harbin 150090, China b College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012, China |
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Abstract: | An automated on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) system was developed for the determination of macrolide antibiotics including erythromycin (ETM), roxithromycin (RTM), tylosin (TLS) and tilmicosin (TMC) in environmental water samples. A Capcell Pak MF Ph-1 column packed with restricted access material (RAM) was used as SPE column for the concentration of the analytes and clean-up of the sample. One milliliter water sample was injected into the conditioned SPE column and the matrix was washed out with 3 mL high purity water. By rotation of the switching valve, macrolides (MLs) were eluted in the back-flush mode and transferred to the analytical column by the chromatographic mobile phase. The matrix effect was evaluated by the directly injection LC-MS and on-line SPE-LC-MS methods. The limits of detection (LODs) and limits of quantification (LOQs) obtained are in the range of 2-6 and 7-20 ng L−1, respectively, which means that the proposed method is suitable for trace analysis of MLs at low level concentration. The intra- and inter-day precisions are in the range of 2.9-7.2% and 3.3-8.9%, respectively. In the three fortified levels (20, 200 and 2000 ng L−1), recoveries of MLs ranging from 86.5% to 98.3% are obtained. |
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Keywords: | Macrolide antibiotics Environmental water Solid-phase extraction Liquid chromatography-tandem mass spectrometry On-line analysis |
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