Simultaneous determination of 12 pharmaceuticals in water samples by ultrasound-assisted dispersive liquid–liquid microextraction coupled with ultra-high performance liquid chromatography with tandem mass spectrometry

Abstract

A new analytical method was developed for simultaneous determination of 12 pharmaceuticals using ultrasound-assisted dispersive liquid-liquid microextraction (DLLME) followed by ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS). Six nonsteroidal anti-inflammatory drugs (NSAIDs, ketoprofen, mefenamic acid, tolfenamic acid, naproxen, sulindac, and piroxicam) and six antibiotics (tinidazole, cefuroxime axetil, ciprofloxacin, sulfamethoxazole, sulfadiazine, and chloramphenicol) were extracted by ultrasound-assisted DLLME using dichloromethane (800 μL) and methanol/acetonitrile (1:1, v/v, 1200 μL) as the extraction and dispersive solvents, respectively. The factors affecting the extraction efficiency, such as the type and volume of extraction and dispersive solvent, vortex and ultrasonic time, sample pH, and ionic strength, were optimized. The ultrasound-assisted process was applied to accelerate the formation of the fine cloudy solution by using a small volume of dispersive solvent, which increased the extraction efficiency and reduced the equilibrium time. Under the optimal conditions, the calibration curves showed good linearity in the range of 0.04-20 ng mL (ciprofloxacin and sulfadiazine), 0.2-100 ng mL (ketoprofen, tinidazole, cefuroxime axetil, naproxen, sulfamethoxazole, and sulindac), and 1-200 ng mL (mefenamic acid, tolfenamic acid, piroxicam, and chloramphenicol). The LODs and LOQs of the method were in the range of 0.006-0.091 and 0.018-0.281 ng mL, respectively. The relative recoveries of the target analytes were in the range from 76.77 to 99.97 % with RSDs between 1.6 and 8.8 %. The developed method was successfully applied to the extraction and analysis of 12 pharmaceuticals in five kinds of water samples (drinking water, running water, river water, influent and effluent wastewater) with satisfactory results. Graphical Abstract Twelve pharmaceuticals in water samples analyted by UHPLC-MS/MS using ultrasound-assisted DLLME.

Prevalence of Vancomycin-Resistant Enterococci and Antimicrobial Residues in Wastewater and Surface Water

“…In most samples of surface water, chloramphenicol was below the LOD. In Shenyang, China, Guan et al determined 297 ng/L in WWTP influent and less than the LOD in river water samples [37], while Li et al reported concentrations from below the LOD to 635 ng/L [38]. Camacho-Munoz et al did not detect chloramphenicol in any samples taken from two WWTPs in Western and Northern Europe [39].…”

Method Optimization: Analysis of Benzbromarone and Tolfenamic Acid in Citrus Tissues and Soil Using Liquid Chromatography Coupled With Triple-Quadrupole Mass Spectrometry

“…While higher sensitivity has been achieved for the detection of tolfenamic acid using a UPLC-MS/MS method with of LOD 0.076 ng/mL and LOQ 0.216 ng/mL in wastewater (Guan et al, 2016), the method required concentration of the samples using solid-phase extraction (SPE) methods. SPE has been reported for the extraction and purification of benzbromarone and tolfenamic acid.…”

“…Detection methods for benzbromarone and tolfenamic acid have been developed for several animal and human tissues as well as wastewater (Beyer et al, 2005;Gallo et al, 2008;Guan et al, 2016) however, methods for the simultaneous analysis of benzbromarone and tolfenamic acid from plant tissue are not available.…”

Carbon and Tin-Based Polyacrylonitrile Hybrid Architecture Solid Phase Microextraction Fiber for the Detection and Quantification of Antibiotic Compounds in Aqueous Environmental Systems

“…Therefore, before using chromatographic or hyphenated techniques sample enrichment is an essential step. The most common sample enrichment techniques to detect antibiotic residues are liquid-liquid extraction (LLE) [23,24], dispersive liquid-liquid microextraction [25,26], solid-phase extraction [27,28], solid-phase microextraction [29,30,31], pressurized liquid extraction [32,33], matrix solid-phase dispersion extraction [34,35], and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method [36,37]. Among these methods, SPME has gained popularity owing to its superior features such as low cost, high extractability, almost solventless uses and easy to operate technique.…”