Trace determination of pharmaceuticals and other wastewater-derived micropollutants by solid phase extraction and gas chromatography/mass spectrometry

Bisceglia, Kevin J.; Yu, Jim; Coelhan, Mehmet; Bouwer, Edward J.; Roberts, A. Lynn

doi:10.1016/j.chroma.2009.11.062

Cited by 80 publications

(43 citation statements)

References 25 publications

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“…EOCs are widely used in consumer goods, such as fragrances, antiseptics, and drugs for human and veterinary application. Pharmaceuticals and personal care products (PPCPs) comprise an interesting group of EOCs that are being continuously released into the environment mainly through wastewater effluents, both treated and untreated [2,3], or run-off from biosolids applied to land [4]. This group includes pharmaceutically active compounds such as analgesics, antiinflammatories, psychiatric drugs, lipid regulators, antibiotics, antiseptics, anticonvulsants…, and personal care products such as fragrances, plasticizers, UV filters, and insect repellents....…”

Section: Introductionmentioning

confidence: 99%

“…Due to their low levels, analytes in samples need to be extracted and concentrated prior to analysis. Most analytical protocols on the extraction of contaminants from aqueous samples (groundwater, surface water, and wastewater) rely on using liquid-liquid extraction (LLE) or solidphase extraction (SPE) [2]. As drawbacks, these techniques generally require large volumes of organic solvents, additional clean-up steps, and extensive sample manipulation.…”

Section: Introductionmentioning

confidence: 99%

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Environmentally friendly analysis of emerging contaminants by pressurized hot water extraction–stir bar sorptive extraction–derivatization and gas chromatography–mass spectrometry

2012

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This work describes the development, optimization, and validation of a new method for the simultaneous determination of a wide range of pharmaceuticals (betablockers, lipid regulators…) and personal care products (fragrances, UV filters, phthalates…) in both aqueous and solid environmental matrices. Target compounds were extracted from sediments using pressurized hot water extraction followed by stir bar sorptive extraction. The first stage was performed at 1,500 psi during three static extraction cycles of 5 min each after optimizing the extraction temperature (50-150°C) and addition of organic modifiers (% methanol) to water, the extraction solvent. Next, aqueous extracts and water samples were processed using polydimethylsiloxane bars. Several parameters were optimized for this technique, including extraction and desorption time, ionic strength, presence of organic modifiers, and pH. Finally, analytes were extracted from the bars by ultrasonic irradiation using a reduced amount of solvent (0.2 mL) prior to derivatization and gas chromatography-mass spectrometry analysis. The optimized protocol uses minimal amounts of organic solvents (<10 mL/sample) and time (≈8 h/sample) compared to previous existing methodologies. Low standard deviation (usually below 10 %) and limits of detection (sub-ppb) vouch for the applicability of the methodology for the analysis of target compounds at trace levels. Once developed, the method was applied to determine concentrations of these compounds in several types of sample (wastewater, seawater, pore water, and sediment) from Cadiz Bay (SW Spain). To our knowledge, these findings represent the first information available on the presence of some of the target compounds in the marine environment.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Environmentally friendly analysis of emerging contaminants by pressurized hot water extraction–stir bar sorptive extraction–derivatization and gas chromatography–mass spectrometry

2012

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“…For example, liquid chromatography coupled with detection by tandem mass spectrometry has been commonly used for detection of trace pharmaceuticals and other wastewater-derived micropollutants (5). Although such methods are very powerful in identifying trace pollutants, cost prohibits their widespread use by environmental researchers and, most importantly, prevents real-time analysis of water quality (6). Other techniques using bench top gas chromatography-mass spectrometry have also been demonstrated as viable methods for detection of basic pharmaceuticals with reduced cost (7).…”

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confidence: 99%

Ultrasensitive detection of waste products in water using fluorescence emission cavity-enhanced spectroscopy

Bixler

Cone

Hokr

et al. 2014

Proc. Natl. Acad. Sci. U.S.A.

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Clean water is paramount to human health. In this article, we present a technique for detection of trace amounts of human or animal waste products in water using fluorescence emission cavity-enhanced spectroscopy. The detection of femtomolar concentrations of urobilin, a metabolic byproduct of heme metabolism that is excreted in both human and animal waste in water, was achieved through the use of an integrating cavity. This technique could allow for real-time assessment of water quality without the need for expensive laboratory equipment.water contamination | fluorescence spectroscopy | femtomolar detection

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“…Numerous methods like titrimetry [4][5][6] , voltammetry 7 , fluorimetry 8 colorimetry 9 , UV-spectrophotometry [10][11] , quantitative thin-layer chromatography (TLC) 10 , high-performance liquid chromatography (HPLC) [12][13][14][15] and gas chromatography (GC) 16 have been reported for the analysis of paracetamol alone and its combinations in pharmaceuticals. Method development is the setting up of an analytical procedure that will be appropriate for the analysis of a particular sample and makes the analysis simpler, sensitive and easier.…”

mentioning

confidence: 99%

Development and Validation of A UV Spectroscopic Method for Analysis of Paracetamol in Bulk Powder and Tablet

Sharma¹,

Pareek²,

Joshi³

et al. 2013

Orientjchem.

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INTRODUCTIONParacetamol or acetaminophen is active metabolites of phenacitin. It is a widely used overthe counter analgesic and antipyretic. Chemically, it is 4-hydroxy acetanilide (acetaminophen) 1 . Paracetamol and other NSAIDs all act by the same mechanism (inhibition of prostaglandin synthesis by inhibiting cyclooxygenase (COX)) and all show varying levels of analgesic, anti-inflammatory, antipyretic and anti-platelet actions 2-3 . Paracetamol is official in Indian Pharmacopoeia and British Pharmacopoeia. Both compendia suggest titrimetric and UV spectrophotometric assay method for paracetamol in bulk and tablet formulations. ORIENTAL JOURNAL OF CHEMISTRY ABSTRACTThe method has been developed and validated for the assay of Paracetamol using mixed solution of methanol and phosphate buffer 6.8 as a solvent in ratio of (1:3) (further diluted in phosphate buffer 6.8 only). The λ max (absorption maxima) of the drug was found to be 246 nm. Linear response was observed in the range of 2-24ìg/ml with a regression coefficient of 0.999. Furthermore various validation parameters as per ICH Q2B guideline were tested and found accordingly. The method and solution was significantly (P<0.05) stable for 15 days. The percent purity (99.09 %) and % Recovery at 80, 100 and 120 % were found to be 102.00±2.027, 102.10±4.913 and 100.00±4.819 respectively for marketed paracetamol tablets. Developed method was a less toxic, cheap, eco-friendly but equally sensitive spectroscopic method for quantitative determination of paracetamol for regular quality control purpose in laboratories.

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Trace determination of pharmaceuticals and other wastewater-derived micropollutants by solid phase extraction and gas chromatography/mass spectrometry

Cited by 80 publications

References 25 publications

Environmentally friendly analysis of emerging contaminants by pressurized hot water extraction–stir bar sorptive extraction–derivatization and gas chromatography–mass spectrometry

Environmentally friendly analysis of emerging contaminants by pressurized hot water extraction–stir bar sorptive extraction–derivatization and gas chromatography–mass spectrometry

Ultrasensitive detection of waste products in water using fluorescence emission cavity-enhanced spectroscopy

Development and Validation of A UV Spectroscopic Method for Analysis of Paracetamol in Bulk Powder and Tablet

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