Beijing Key Laboratory of Water Resources and Environmental Engineering, School of Water Resources and Environment, China University of Geosciences, Beijing, 100083, People's Republic of China.
Environ Sci Pollut Res Int. 2015 Nov;22(21):16857-67. doi: 10.1007/s11356-015-4900-1. Epub 2015 Jun 24.
An optimized solid-phase extraction (SPE) and ultra-high performance liquid chromatography-electrospray tandem mass spectrometry (UPLC-MS/MS) method was developed for the effective analysis of 35 antibiotics including sulfonamides (SAs), quinolones (QLs), tetracyclines (TCs), macrolides (MALs), lincomycin (LIN), and chloramphenicol (CAP). The addition of 0.1% formic acid to the mobile phase was favorable for the formation of M + H and the enhancement in the detection signals, but using ammonium formate decreased M + H with a corresponding reduction in the response of CAP. The optimal pH range for the SPE was 4.5 ∼ 5.0 with 6 mL aqueous ammonia/methanol (5/95, v/v) as the optimized eluent. An internal standard (IS) was selected for each type of analytes based on similarities in classification and retention time. The detection was completed in less than 10 min and was excellent with method detection limits (MDL) of 0.29 ∼ 4.03 ng/L. The recoveries of the antibiotics in samples from ultrapure water and groundwater were 67.13 ∼ 93.00% and 68.91 ∼ 92.67%, respectively. The antibiotics in samples collected from wastewater, surface water, and groundwater were also effectively detected. This newly developed method has the advantages of short detection times, small sample consumption, excellent reproducibility, and high sensitivity. This provides a reliable and promising technique for the simultaneous detection and monitoring of various residual antibiotics in aqueous environmental samples.
建立了一种优化的固相萃取（SPE）和超高效液相色谱-电喷雾串联质谱（UPLC-MS/MS）方法，用于有效分析 35 种抗生素，包括磺胺类（SAs）、喹诺酮类（QLs）、四环素类（TCs）、大环内酯类（MALs）、林可霉素（LIN）和氯霉素（CAP）。在流动相中添加 0.1%甲酸有利于[M+H]+的形成和检测信号的增强，但使用甲酸铵会降低[M+H]+，同时 CAP 的响应也会相应降低。SPE 的最佳 pH 范围为 4.5∼5.0，6 mL 氨水/甲醇（5/95，v/v）作为优化洗脱液。根据分类和保留时间的相似性，为每种类型的分析物选择了内标（IS）。检测在不到 10 分钟内完成，方法检测限（MDL）为 0.29∼4.03 ng/L，效果极好。超纯水和地下水样品中抗生素的回收率分别为 67.13∼93.00%和 68.91∼92.67%。废水、地表水和地下水样品中的抗生素也得到了有效检测。该新方法具有检测时间短、样品消耗少、重现性好、灵敏度高等优点。为同时检测和监测水环环境样品中各种残留抗生素提供了一种可靠、有前景的技术。
