ABSTRACT
A sensitive yet robust analytical method is presented for the simultaneous determination of 12 human pharmaceuticals (valproic acid, phenytoin, ibuprofen, gabapentin, acetaminophen, gemfibrozil, naproxen, ketoprofen, secobarbital, phenobarbital, 5-fluorouracil, and diclofenac) and 6 antiseptics (biosol, biphenylol, p-chloro-m-cresol, p-chloro-m-xylenol, chlorophene, and triclosan). The method employs solid-phase extraction (SPE) followed by a novel pentafluorobenzylation using a mixture of acetontrile/water (1/1, v/v). The method is simple to perform (derivatization can be completed in a single test tube) and eliminates the need for any solvent/SPE cartridge drying or blow-down. It affords excellent resolution, high sensitivity and reproducibility, and freedom from interference even for matrices as complex as untreated sewage. The method was applied to the analysis of sewage samples using 15 isotopically labeled surrogates, which resulted in the detection of 10 of the 12 pharmaceuticals and all of the antiseptics sought. Ten of 15 surrogates were synthesized from pure analytes by a simple H-D exchange reaction employing D(2)O and D(2)SO(4). Measured recoveries were sensitive to matrix effects and varied substantially among analytes, indicative of the limitations associated with using a single surrogate standard.
Subject(s)
Anti-Infective Agents, Local/analysis , Gas Chromatography-Mass Spectrometry/methods , Pharmaceutical Preparations/analysis , Solid Phase Extraction/methods , Water Pollutants, Chemical/analysis , Anti-Infective Agents, Local/isolation & purification , Fluorobenzenes/chemistry , Indicator Dilution Techniques , Pharmaceutical Preparations/isolation & purification , Sewage/chemistry , Water Pollutants, Chemical/isolation & purificationABSTRACT
The presence of pharmaceuticals and other wastewater-derived micropollutants in surface and groundwaters is receiving intense public and scientific attention. Yet simple GC/MS methods that would enable measurement of a wide range of such compounds are scarce. This paper describes a GC/MS method for the simultaneous determination of 13 pharmaceuticals (acetaminophen, albuterol, allopurinol, amitriptyline, brompheniramine, carbamazepine, carisoprodol, ciclopirox, diazepam, fenofibrate, metoprolol, primidone, and terbinafine) and 5 wastewater-derived contaminants (caffeine, diethyltoluamide, n-butylbenzene sulfonamide, n-nonylphenol, and n-octylphenol) by solid phase extraction (SPE) and derivatization with BSTFA. The method was applied to the analysis of raw and treated sewage samples obtained from a wastewater treatment plant located in the mid-Atlantic United States. All analytes were detected in untreated sewage, and 14 of the 18 analytes were detected in treated sewage.
Subject(s)
Gas Chromatography-Mass Spectrometry/methods , Pharmaceutical Preparations/analysis , Sewage/analysis , Solid Phase Extraction/methods , Water Pollutants, Chemical/analysis , Hydrogen-Ion Concentration , Pharmaceutical Preparations/isolation & purification , Sensitivity and Specificity , Solvents , Waste Disposal, Fluid/methods , Water Pollutants, Chemical/isolation & purificationABSTRACT
Pharmaceuticals and personal care products (PPCPs) have been the focus of much recent research as concerns rise about their occurrence in bodies of water worldwide. In an effort to characterize the risk and determine the prevalence of these micropollutants in lakes and rivers, many researchers are examining PPCP removal from impaired water during wastewater treatment and water recycling (soil passage) processes. Biodegradation studies and projects considering combinations of biodegradation and other removal processes have been conducted over a wide range of compound categories and therapeutic classes, as well as across different systems and scales of study. This review summarizes the extent of PPCP removal observed in these various systems.
