Determination of multiple pharmaceutical classes in surface and ground waters by liquid chromatography-ion trap-tandem mass spectrometry
Само за регистроване кориснике
2009
Чланак у часопису (Објављена верзија)
Метаподаци
Приказ свих података о документуАпстракт
This paper describes development, optimization and application of analytical method for determination and reliable confirmation of nineteen pharmaceuticals from different therapeutic classes (antibiotics-beta-lactams. cephalosporines, sulfonamides, macrolides and tetracyclines: benzodiazepines; antiepileptics and analgoantipyretics) in surface and ground waters at ng l(-1) levels. Water samples were prepared using solid-phase extraction and extracts were analyzed by liquid chromatography-ion trap-tandem mass spectrometry with electrospray ionization in both positive and negative ionization mode. The efficiency of ten different SPE cartridges to extract diverse Compounds from water was tested. The pH-value of the water sample, the volume of elution solvent and the sample volume were optimized. Matrix effect, especially pronounced for cephalexin and metamizole, was eliminated using matrix-matched standards. It was determined that extraction should be performed at pH similar to 7.5, i.e. ...without pH adjustment, and at pH 3, depending on the analyte. Azithromycin, doxycycline and acetylsalicylic acid must be extracted in acidic environment, whereas extraction of paracetamol, ampicillin, erythromycin and metamizole should be performed without pH adjustment. Repeatability of the method was generally lower than 20%. The estimated limits of detection were in the range from 0.15 to 12.46 ng l(-1). The method was applied to 26 water samples for monitoring of selected drug residues. Results revealed the presence of carbamazepine (80% of water samples), azithromycin (23%), as well as trimethoprim and paracetamol (both 15%). The most striking was the false positive signal of diclofenac in every analyzed water sample. Confirmation of the positive results was performed by repeated injection of the positive sample extracts using confirmatory method with additional transitions.
Кључне речи:
Multiclass pharmaceuticals / Antibiotics / Liquid chromatography-tandem mass spectrometry / Ion trap / Solid-phase extraction / Water analysisИзвор:
Journal of Chromatography A, 2009, 1216, 25, 4989-5000Издавач:
- Elsevier Science Bv, Amsterdam
Финансирање / пројекти:
- Развој метода за сепарацију, предконцентрисање, одређивање и уклањање загађивача околине (RS-MESTD-MPN2006-2010-142002)
DOI: 10.1016/j.chroma.2009.04.059
ISSN: 0021-9673
PubMed: 19426985
WoS: 000267086400008
Scopus: 2-s2.0-65649141661
Институција/група
Tehnološko-metalurški fakultetTY - JOUR AU - Grujić, Svetlana AU - Vasiljević, Tatjana AU - Laušević, Mila PY - 2009 UR - http://TechnoRep.tmf.bg.ac.rs/handle/123456789/1505 AB - This paper describes development, optimization and application of analytical method for determination and reliable confirmation of nineteen pharmaceuticals from different therapeutic classes (antibiotics-beta-lactams. cephalosporines, sulfonamides, macrolides and tetracyclines: benzodiazepines; antiepileptics and analgoantipyretics) in surface and ground waters at ng l(-1) levels. Water samples were prepared using solid-phase extraction and extracts were analyzed by liquid chromatography-ion trap-tandem mass spectrometry with electrospray ionization in both positive and negative ionization mode. The efficiency of ten different SPE cartridges to extract diverse Compounds from water was tested. The pH-value of the water sample, the volume of elution solvent and the sample volume were optimized. Matrix effect, especially pronounced for cephalexin and metamizole, was eliminated using matrix-matched standards. It was determined that extraction should be performed at pH similar to 7.5, i.e. without pH adjustment, and at pH 3, depending on the analyte. Azithromycin, doxycycline and acetylsalicylic acid must be extracted in acidic environment, whereas extraction of paracetamol, ampicillin, erythromycin and metamizole should be performed without pH adjustment. Repeatability of the method was generally lower than 20%. The estimated limits of detection were in the range from 0.15 to 12.46 ng l(-1). The method was applied to 26 water samples for monitoring of selected drug residues. Results revealed the presence of carbamazepine (80% of water samples), azithromycin (23%), as well as trimethoprim and paracetamol (both 15%). The most striking was the false positive signal of diclofenac in every analyzed water sample. Confirmation of the positive results was performed by repeated injection of the positive sample extracts using confirmatory method with additional transitions. PB - Elsevier Science Bv, Amsterdam T2 - Journal of Chromatography A T1 - Determination of multiple pharmaceutical classes in surface and ground waters by liquid chromatography-ion trap-tandem mass spectrometry EP - 5000 IS - 25 SP - 4989 VL - 1216 DO - 10.1016/j.chroma.2009.04.059 ER -
@article{ author = "Grujić, Svetlana and Vasiljević, Tatjana and Laušević, Mila", year = "2009", abstract = "This paper describes development, optimization and application of analytical method for determination and reliable confirmation of nineteen pharmaceuticals from different therapeutic classes (antibiotics-beta-lactams. cephalosporines, sulfonamides, macrolides and tetracyclines: benzodiazepines; antiepileptics and analgoantipyretics) in surface and ground waters at ng l(-1) levels. Water samples were prepared using solid-phase extraction and extracts were analyzed by liquid chromatography-ion trap-tandem mass spectrometry with electrospray ionization in both positive and negative ionization mode. The efficiency of ten different SPE cartridges to extract diverse Compounds from water was tested. The pH-value of the water sample, the volume of elution solvent and the sample volume were optimized. Matrix effect, especially pronounced for cephalexin and metamizole, was eliminated using matrix-matched standards. It was determined that extraction should be performed at pH similar to 7.5, i.e. without pH adjustment, and at pH 3, depending on the analyte. Azithromycin, doxycycline and acetylsalicylic acid must be extracted in acidic environment, whereas extraction of paracetamol, ampicillin, erythromycin and metamizole should be performed without pH adjustment. Repeatability of the method was generally lower than 20%. The estimated limits of detection were in the range from 0.15 to 12.46 ng l(-1). The method was applied to 26 water samples for monitoring of selected drug residues. Results revealed the presence of carbamazepine (80% of water samples), azithromycin (23%), as well as trimethoprim and paracetamol (both 15%). The most striking was the false positive signal of diclofenac in every analyzed water sample. Confirmation of the positive results was performed by repeated injection of the positive sample extracts using confirmatory method with additional transitions.", publisher = "Elsevier Science Bv, Amsterdam", journal = "Journal of Chromatography A", title = "Determination of multiple pharmaceutical classes in surface and ground waters by liquid chromatography-ion trap-tandem mass spectrometry", pages = "5000-4989", number = "25", volume = "1216", doi = "10.1016/j.chroma.2009.04.059" }
Grujić, S., Vasiljević, T.,& Laušević, M.. (2009). Determination of multiple pharmaceutical classes in surface and ground waters by liquid chromatography-ion trap-tandem mass spectrometry. in Journal of Chromatography A Elsevier Science Bv, Amsterdam., 1216(25), 4989-5000. https://doi.org/10.1016/j.chroma.2009.04.059
Grujić S, Vasiljević T, Laušević M. Determination of multiple pharmaceutical classes in surface and ground waters by liquid chromatography-ion trap-tandem mass spectrometry. in Journal of Chromatography A. 2009;1216(25):4989-5000. doi:10.1016/j.chroma.2009.04.059 .
Grujić, Svetlana, Vasiljević, Tatjana, Laušević, Mila, "Determination of multiple pharmaceutical classes in surface and ground waters by liquid chromatography-ion trap-tandem mass spectrometry" in Journal of Chromatography A, 1216, no. 25 (2009):4989-5000, https://doi.org/10.1016/j.chroma.2009.04.059 . .