Premium
Determination of sedative hypnotics in sewage sludge by pressurized liquid extraction with high‐performance liquid chromatography and tandem mass spectrometry
Author(s) -
Arbeláez Paula,
Granados Judith,
Borrull Francesc,
Marcé Rosa Maria,
Pocurull Eva
Publication year - 2014
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201400791
Subject(s) - chromatography , chemistry , extraction (chemistry) , repeatability , liquid chromatography–mass spectrometry , mass spectrometry , sewage sludge , high performance liquid chromatography , tandem mass spectrometry , sewage , waste management , engineering
This paper describes a method for the determination of eight sedative hypnotics (benzodiazepines and barbiturates) in sewage sludge using pressurized liquid extraction and liquid chromatography with tandem mass spectrometry. Pressurized liquid extraction operating conditions were optimized and maximum recoveries were reached using methanol under the following operational conditions: 100ºC, 1500 psi, extraction time of 5 min, one extraction cycle, flush volume of 60% and purge time of 120 s. Pressurized liquid extraction recoveries were higher than 88% for all the compounds except for carbamazepine (55%). The repeatability and reproducibility between days, expressed as relative standard deviation ( n = 5), were lower than 6 and 10%, respectively. The detection limits for all compounds were lower than 12.5 μg/kg of dry weight. The method was applied to determine benzodiazepines and barbiturates in sewage sludge from urban sewage treatment plants, and carbamazepine showed the highest concentration (7.9–18.9 μg/kg dry weight).