Ultra performance liquid chromatography tandem mass spectrometry performance evaluation for analysis of antibiotics in natural waters

Abstract

An ultra performance liquid chromatography electrospray tandem mass spectrometry (UPLC/MS/MS) method was developed and validated for the determination of 17 antibiotics in natural waters in one single extraction and chromatographic procedure. Gradient separation conditions were optimised for 17 compounds belonging to five different antibiotic groups: quinolones (oxolinic acid, nalidixic acid, pipemidic acid, flumequine), fluoroquinolones (enoxacin, ciprofloxacin, norfloxacin, ofloxacin, enrofloxacin, sarafloxacin, danofloxacin, difloxacin, lomefloxacin), sulphonamides (sulphamethoxazole, sulphamethazine), nitro-imidazole (ornidazole) and diaminopyrimidine (trimethoprim). The separation of all compounds, obtained using a 1.7 microm particle size column (100 mm x 2.1 mm), was achieved within 10 min time. Water samples were adjusted to pH 7 and extracted using Oasis hydrophilic-lipophilic balance (HLB) solid phase extraction cartridges. After elution with methanol and concentration, extracts were injected in a C18 column (Acquity UPLC BEH C18) and detected by tandem mass spectrometry. Average recovery from 100 ng L(-1) fortified samples was higher than 70% for most of the compounds, with relative standard deviations below 20%. Performances of the method (recoveries, detection limit, quantification limit and relative standard deviation) and matrix effects were studied, and results obtained showed that method was suitable for routine analysis of antibiotics in surface water. Samples analysis from Seine River (France) confirmed the interest of antibiotic contamination evaluation in that area.

Contamination levels of human pharmaceutical compounds in French surface and drinking water

“…25 mL of fenuron at 10 mg L À1 was added before extraction. The extraction and analytical procedures were adapted from Tamtam et al 38 A single extraction-separationdetection procedure was developed for the analysis of the 20 HPCs in SW and DW.…”

Simultaneous determination of human and veterinary antibiotics in various environmental matrices by rapid resolution liquid chromatography–electrospray ionization tandem mass spectrometry

“…The most frequently used extraction methods for water samples were solid phase extraction (SPE) with different cartridges and conditions [10,[26][27][28][29][30][31][32]. To reduce matrix effect of complex coextracted components in wastewater matrices in instrumental analysis, cleanup steps used included: decreasing sample volume, MAX/MCX cartridge cleanup after HLB extraction [29,33], SAX-HLB tandem cartridges [10], and silica SPE cartridge cleanup after HLB extraction [28].…”

“…Antibiotics in environmental matrices have been analyzed by liquid chromatography (LC) with diode-array detection (DAD) [47,48], fluorescence detection (FLD) [47], mass spectrometry detection (MS) [44], or tandem MS (LC-MS/MS) using ion-trap MS or triple quadrupole MS [10,30,32,41,49]. LC-MS/MS is considered the preferred method for routine analysis of antibiotics in complex environmental samples because of its sensitivity and selectivity comparing to LC-DAD, LC-FLD, and LC-MS [50].…”

Trends in the occurrence of human and veterinary antibiotics in the sediments of the Yellow River, Hai River and Liao River in northern China

“…Various antibiotics have been frequently detected in surface water, ground water, even drinking water (Hirsch et al, 1999;Kolpin et al, 2002;Kim and Carlson, 2007;Xu et al, 2007b;Barnes et al, 2008;Focazio et al, 2008;Fick et al, 2009;Tamtam et al, 2009;Xu et al, 2009;Yang et al, 2011). The concentrations of sulfonamide and macrolide antibiotics in water were found even up to mg/L (Hirsch et al,1999;Yang et al, 2011).…”

“…Moreover, environmental water samples collected proximal to pharmaceutical manufacturing facilities were found to have milligram per liter concentrations of antibiotics including cetirizine, ciprofloxacin, norfloxacin and enoxacin (Fick et al, 2009). But most of the measured fluoroquinolones and tetracyclines in water were found at much lower concentration levels (mostly ng/L) or not detected (Hirsch et al, 1999;Kim and Carlson, 2007;Xu et al, 2007b;Tamtam et al, 2009;Xu et al, 2009;Yang et al, 2011).…”