Sensitive determination of illicit drugs in wastewater using enrichment bag-based liquid-phase microextraction and liquid-chromatography tandem mass spectrometry

There is no author summary for this article yet. Authors can add summaries to their articles on ScienceOpen to make them more accessible to a non-specialist audience.

Abstract

To concentrate trace level of analytes in complex wastewater, sample preparation is necessary prior to instrumental analysis. In this work, an enrichment bag-based liquid-phase microextraction (EB-LPME) system was therefore proposed for the first time to isolate and enrich the illicit drugs (amphetamine, methamphetamine, 3,4-methylenedioxymethamphetamine (MDMA), ketamine, codeine and fentanyl) from wastewater. Under the optimum EB-LPME conditions, the recoveries of the model illicit drugs were 40-93% with enrichment factors up to 93. The optimized EB-LPME was compared to hollow fiber-LPME (HF-LPME) in terms of the thickness of the supported liquid membrane (SLM), the effective SLM area, extraction recovery and mass transfer flux. Compared with HF-LPME, EB-LPME possesses larger effective SLM area, and provided higher extraction recovery. In addition, EB-LPME provided larger mass transfer flux than HF-LPME, which was mainly due to the differences in SLM thickness. Therefore, SLM thickness was identified as the main mass transfer flux-determining factor experimentally. The matrix effect of EB-LPME was evaluated using liquid chromatography-tandem mass spectrometry (LC-MS/MS), and excellent sample clean-up was confirmed. Subsequently, EB-LPME-LC-MS/MS was validated with satisfactory results, and the detection of limit of the proposed method was in the range of 0.3-8.7 ng/L. Finally, with standard addition method, EB-LPME-LC-MS/MS was successfully applied for the determination of the model drugs in a local hospital wastewater from Wuhan, China. This study clearly showed that EB-LPME displayed great potential as an efficient sample preparation method for isolation and enrichment of the drugs/pollutants from complex environmental samples for wastewater-based epidemiology in the near future.

Related collections

Most cited references 50

Record: found
Abstract: found
Article: not found

Liquid-liquid-liquid microextraction for sample preparation of biological fluids prior to capillary electrophoresis.

S Pedersen-Bjergaard, K Rasmussen (1999)

Methamphetamine as a model compound was extracted from 2.5-mL aqueous samples adjusted to pH 13 (donor solution) through a thin phase of 1-octanol inside the pores of a polypropylene hollow fiber and finally into a 25-microL acidic acceptor solution inside the hollow fiber. Following this liquid-liquid-liquid microextraction (LLLME), the acceptor solutions were analyzed by capillary zone electrophoresis (CE). Extractions were performed in simple disposable devices each consisting of a conventional 4-mL sample vial, two needles for introduction and collection of the acceptor solution, and a 8-cm piece of a porous polypropylene hollow fiber. From 5 to 20 different samples were extracted in parallel for 45 min, providing a high sample capacity. Methamphetamine was preconcentrated by a factor of 75 from aqueous standard solutions, human urine, and human plasma utilizing 10(-1) M HCl as the acceptor phase and 10(-1) M NaOH in the donor solution. In addition to preconcentration, LLLME also served as a technique for sample cleanup since large molecules, acidic compounds, and neutral components were not extracted into the acceptor phase. Utilizing diphenhydramine hydrochloride as internal standard, repetitive extractions varied less than 5.2% RSD (n = 6), while the calibration curve for methamphetamine was linear within the range 20 ng/microL to 10 micrograms/mL (r = 0.9983). The detection limit of methamphetamine utilizing LLLME/CE was 5 ng/mL (S/N = 3) in both human urine and plasma.

0 comments Cited 128 times – based on 0 reviews      Review now

Bookmark

Record: found
Abstract: found
Article: not found

Determination of pharmaceuticals of various therapeutic classes by solid-phase extraction and liquid chromatography-tandem mass spectrometry analysis in hospital effluent wastewaters.

Damià Barceló, R Alba, Mira Petrovic … (2006)

A multi-residue analytical method has been developed and validated for determining a selection of 16 pharmaceuticals: the anti-epileptic carbamazepine, seven analgesic/anti-inflammatory drugs (mefenamic acid, indomethacine, ibuprofen, naproxen, diclofenac, ketorolac and acetaminophen), the analgesic opiate codeine, two antidepressants (fluoxetine and paroxetine), beta-blockers (atenolol and propranolol), antibiotic (trimethoprim, metronidazole, and erythromycin) and the anti-ulcer ranitidine in hospital effluent wastewaters. The method allows simultaneous extraction of the pharmaceuticals compounds by solid-phase extraction (SPE) using the Waters Oasis HLB at pH 7. The analytes were then identified and quantitatively determined by liquid chromatography-tandem mass spectrometry (LC-MS-MS) using multiple reaction monitoring (MRM). Recoveries of the pharmaceuticals were higher than 75%, with the exception of ranitidine (45%) and the overall variability of the method was below 9%. The instrumental detection limit (IDL) varied between 2 and 31 pg injected, the method detection limit (LOD) was between 7 and 47 ng/L in spiked hospital effluent. The precision of the method, calculated as relative standard deviation (RSD), ranged from 0.3 to 4.9%. A detail study off matrix effect is included in this work, regarding to signal suppression in these effluent wastewaters from a hospital complex samples. The developed analytical method was applied for preliminary data results in effluent wastewaters from a hospital.