An optimized SPE-LC-MS/MS method for antibiotics residue analysis in ground, surface and treated water samples by response surface methodology- central composite design

Abstract

BackgroundAntibiotic residues are being constantly identified in environmental waters at low concentration. Growing concern has been expressed over the adverse environmental and human health effects even at low concentration. Hence, it is crucial to develop a multi-residues analytical method for antibiotics to generate a considerable dataset which are necessary in the assessment of aquatic toxicity of environmental waters for aquatic organisms and human health. This work aimed to develop a reliable and sensitive multi-residue method based on high performance liquid chromatography coupled with quadrupole-linear ion trap tandem mass spectrometry (HPLC-MS-MS). The method was optimized and validated for simultaneous determination of four classes of antibiotics including, β-lactam, macrolide, fluoroquinolone and nitro-imidazole in treated, ground and surface water matrices.MethodsIn order to optimize the solid phase extraction process, main parameters influencing the extraction process including, pH, the volume of elution solvent and the amount of Na4EDTA were evaluated. The optimization of extraction process was carried out by response surface methodology using central composite design. Analysis of variance was performed for nine target antibiotics using response surface methodology.ResultsThe extraction recoveries were found to be sensitive to the independent variables of pH, the volume of elution solvent and the amount of Na4EDTA. The extraction process was pH-dependent and pH was a significant model term in the extraction process of all target antibiotics. Method validation was performed in optimum operation conditions in which the recoveries were obtained in the range of 50–117% for seven antibiotics in spiked treated and ground water samples and for six antibiotics in spiked river water samples. Method validation parameters in terms of method detection limit were obtained in the range of 1–10 ng/L in treated water, 0.8–10 ng/L in the ground water and 0.8–25 ng/L in river water, linearity varied from 0.95 to 0.99 and repeatability in term of relative standard deviation values was achieved less than 10% with the exception for metronidazole and ceftriaxone. The developed method was applied to the analysis of target antibiotics in treated, ground and surface water samples.ConclusionsTarget antibiotics were analyzed in different water matrices including treated, ground and river water. Seven out of nine antibiotics were detected in Kan River and Firozabad Ditch water samples, although none of them were detected in treated water and ground water samples.Electronic supplementary materialThe online version of this article (10.1186/s40201-017-0282-2) contains supplementary material, which is available to authorized users.

Development and Validation of a LC-MS/MS Method for Determination of Multi-Class Antibiotic Residues in Aquaculture and River Waters, and Photocatalytic Degradation of Antibiotics by TiO2 Nanomaterials

“…For the third process, prior to use of Strata-X or HLB cartridges, an addition of 0.3% Na 2 EDTA reduced the matrix effects and slightly enhanced the recovery yields. Indeed, the third procedure offered high recovery yields for all the antibiotics (89.3-107.4%), whose results were comparable to previous works [19][20][21][23][24][25][27][28][29][30]70,72,74,75], but it required a long sample preparation time of 40 min/sample. Briefly, higher cost and longer sample preparation time were the main drawbacks of the second and the third procedures, compared to the first process, which had a short preparation time of 10 min/sample and was 60% cheaper (Figures S22-S25 in SM).…”

“…The separation was achieved by using a ternary gradient mobile phase consisting of ACN (A), MeOH (B), and water with 0.1% formic acid (C). The total required time for the chromatographic analysis was 20 min, which was comparable or shorter than the time spent of 20-40 min in [27,31,32]. The optimal conditions are listed in Table 2 and presented in Figure 1.…”

Towards the Removal of Antibiotics Detected in Wastewaters in the POCTEFA Territory: Occurrence and TiO2 Photocatalytic Pilot-Scale Plant Performance

“…According to EPA 1694, the filtration of the samples is necessary in order to remove suspension solids. Two filtration steps were carried out prior to analysis using glass fiber filters (1.6 µm, supplied by GVS) for the first filtration stage and nylon filters (0.45 µm, supplied by GVS) for the second stage, as suggested in other research works [33][34][35].…”

Simultaneous Determination of Pharmaceuticals by Solid-phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry: A Case Study from Sharjah Sewage Treatment Plant

“…The simultaneous determination of pharmaceuticals in wastewater is a challenging task due to the variation in their physicochemical properties, their low concentrations, and complexity of the environmental matrices [19,20,21,22,23,24,25]. Based on the literature surveys regarding the most commonly prescribed medications in the Emirate of Sharjah, it was found that the percentage of prescribing antibiotics to treat different types of infections was 45% [26].…”