Optimization of a Solid-Phase Extraction Coupled with a High-Performance Liquid Chromatography and Diode Array Ultraviolet Detection Method for Monitoring of Different Antibiotic Class Residues in Water Samples

色谱法 高效液相色谱法 固相萃取 检出限 色谱检测器 丹诺沙星 化学 材料科学 环丙沙星 抗生素 恩诺沙星 生物化学
作者
Reyad Mahmoud,Ghada M. Hadad,Randa A. Abdel Salam,Hatem I. Mokhtar
出处
期刊:Journal of AOAC International [Oxford University Press]
卷期号:107 (1): 52-60 被引量:1
标识
DOI:10.1093/jaoacint/qsad111
摘要

Abstract Background The increased use of cephalosporin antibiotics in the last few years as well as the detection of their residues in wastewater treatment plants and hospital wastewater poses a risk for infiltration of their residues into environmental water samples. Objective A simplified, sensitive, and convenient solid-phase extraction (SPE) procedure coupled with either HPLC or fast HPLC methods with diode array detection was developed and validated to screen the residues of six different cephalosporin antibiotics: cefoperazone, cefipime, ceftazedime, ceftriaxone, cefdinir, and cefotaxime, along with amoxicillin, levofloxacin, and ciprofloxacin in water samples. Methods An HPLC–diode array detector (HPLC–DAD) method and a fast HPLC method, based on a core-shell stationary phase, were developed for the fast screening of the antibiotic compounds. In addition, the SPE step was optimized to enable the extraction of the studied drugs with high accuracy of the recovered amounts of residues. Results The method sensitivity was enhanced by the coupling of SPE with HPLC–DAD and fast HPLC to achieve low LODs; from 0.2 to 3.8 ng/mL and from 0.65 to 12.2 ng/mL, respectively. The developed methods were augmented by LC–MS/MS determination for confirmation of identity and quantity of any positively identified sample. The method was applied to the analysis of water samples collected from a rural site. In Addition, an example application of cleaning validation of cefotaxime-contaminated stainless-steel surfaces was provided. Conclusion The method’s simplicity and high sensitivity encourage its application in monitoring of antibiotic residues in different types of water samples such as environmental samples and samples from cleaning validation activities. Highlights HPLC–DAD and fast HPLC methods were developed for separation of nine different antibiotics. The combination with the SPE procedure achieved low detection limits; from 0.2 to 3.8 ng/mL for SPE–HPLC–DAD and from 0.65 to 12.2 ng/mL for SPE–fast HPLC.
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