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One step solvent bar microextraction and derivatization followed by gas chromatography-mass spectrometry for the determination of pharmaceutically active compounds in drain water samples.
J Chromatogr A. 2012 Apr 27; 1235:26-33.JC

Abstract

For the first time, a simple and novel one-step combined solvent bar microextraction with derivatization with GC-MS analysis, was developed for the determination of pharmaceutically active compounds (PhACs) in water samples. In the procedure, the derivatization reagent was added in the extraction solvent (solvent bar), so that the analytes could be extracted from the aqueous sample and simultaneously derivatized in the solvent bar to enhance their volatility and improve chromatographic performance. After extraction, the derivatized analytes in the extract were directly injected into a GC-MS system for analysis. Six PhACs including naproxen, ibuprofen, ketoprofen, propranolol, diclofenac, and alprenolol were used here to develop and evaluate the method. The parameters affecting the derivatization and extraction efficiency including derivatization time and temperature, the proportion of derivatization reagent, the type of organic solvent, extraction time, extraction temperature, pH of sample solution, effect of ionic strength, and sample agitation speed, were investigated in detail. Under the most favorable conditions, the method provided good limits of detection ranging from 0.006 to 0.022 μg/L, linearity (from 0.1-50 to 0.2-50 μg/L, depending on analytes) and repeatability of extractions (RSDs below 9.5%, n=5). The proposed method was compared to hollow fiber protected liquid-phase microextraction and solid-phase microextraction, and showed higher extraction efficiency and/or shorter extraction time. The proposed method was applied to the determination of six PhACs in drain water, and was demonstrated to be simple, fast and efficient.

Authors+Show Affiliations

Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.No affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't
Validation Study

Language

eng

PubMed ID

22436669

Citation

Guo, Liang, and Hian Kee Lee. "One Step Solvent Bar Microextraction and Derivatization Followed By Gas Chromatography-mass Spectrometry for the Determination of Pharmaceutically Active Compounds in Drain Water Samples." Journal of Chromatography. A, vol. 1235, 2012, pp. 26-33.
Guo L, Lee HK. One step solvent bar microextraction and derivatization followed by gas chromatography-mass spectrometry for the determination of pharmaceutically active compounds in drain water samples. J Chromatogr A. 2012;1235:26-33.
Guo, L., & Lee, H. K. (2012). One step solvent bar microextraction and derivatization followed by gas chromatography-mass spectrometry for the determination of pharmaceutically active compounds in drain water samples. Journal of Chromatography. A, 1235, 26-33. https://doi.org/10.1016/j.chroma.2012.02.068
Guo L, Lee HK. One Step Solvent Bar Microextraction and Derivatization Followed By Gas Chromatography-mass Spectrometry for the Determination of Pharmaceutically Active Compounds in Drain Water Samples. J Chromatogr A. 2012 Apr 27;1235:26-33. PubMed PMID: 22436669.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - One step solvent bar microextraction and derivatization followed by gas chromatography-mass spectrometry for the determination of pharmaceutically active compounds in drain water samples. AU - Guo,Liang, AU - Lee,Hian Kee, Y1 - 2012/03/05/ PY - 2012/01/05/received PY - 2012/02/27/revised PY - 2012/02/28/accepted PY - 2012/3/23/entrez PY - 2012/3/23/pubmed PY - 2012/5/23/medline SP - 26 EP - 33 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1235 N2 - For the first time, a simple and novel one-step combined solvent bar microextraction with derivatization with GC-MS analysis, was developed for the determination of pharmaceutically active compounds (PhACs) in water samples. In the procedure, the derivatization reagent was added in the extraction solvent (solvent bar), so that the analytes could be extracted from the aqueous sample and simultaneously derivatized in the solvent bar to enhance their volatility and improve chromatographic performance. After extraction, the derivatized analytes in the extract were directly injected into a GC-MS system for analysis. Six PhACs including naproxen, ibuprofen, ketoprofen, propranolol, diclofenac, and alprenolol were used here to develop and evaluate the method. The parameters affecting the derivatization and extraction efficiency including derivatization time and temperature, the proportion of derivatization reagent, the type of organic solvent, extraction time, extraction temperature, pH of sample solution, effect of ionic strength, and sample agitation speed, were investigated in detail. Under the most favorable conditions, the method provided good limits of detection ranging from 0.006 to 0.022 μg/L, linearity (from 0.1-50 to 0.2-50 μg/L, depending on analytes) and repeatability of extractions (RSDs below 9.5%, n=5). The proposed method was compared to hollow fiber protected liquid-phase microextraction and solid-phase microextraction, and showed higher extraction efficiency and/or shorter extraction time. The proposed method was applied to the determination of six PhACs in drain water, and was demonstrated to be simple, fast and efficient. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/22436669/One_step_solvent_bar_microextraction_and_derivatization_followed_by_gas_chromatography_mass_spectrometry_for_the_determination_of_pharmaceutically_active_compounds_in_drain_water_samples_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(12)00374-3 DB - PRIME DP - Unbound Medicine ER -