New micro-solid phase extraction techniques based on mesoporous materials for selected antibiotic and antifungal agents

New microextraction techniques have been developed for sample preparation of azole drugs and penicillins in water, milk and biological samples prior to their liquid chromatographic determination. A microextraction method based on solid phase membrane tip extraction (SPMTE) incorporated with mesoporo...

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Main Author:	Yahaya, Noorfatimah
Format:	Thesis
Language:	English
Published:	2014
Subjects:	QD Chemistry
Online Access:	http://eprints.utm.my/id/eprint/78300/1/NoorfatimahYahayaPFS2014.pdf
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spelling	my-utm-ep.783002018-08-12T03:49:02Z New micro-solid phase extraction techniques based on mesoporous materials for selected antibiotic and antifungal agents 2014-06 Yahaya, Noorfatimah QD Chemistry New microextraction techniques have been developed for sample preparation of azole drugs and penicillins in water, milk and biological samples prior to their liquid chromatographic determination. A microextraction method based on solid phase membrane tip extraction (SPMTE) incorporated with mesoporous silica, MCM-41, was developed for the determination of azole antifungal drugs, namely voriconazole (VRZ), ketoconazole (KTZ) and itraconazole (ITZ) in human plasma. Under the optimized conditions, the method demonstrated good linearity (r2 = 0.9958) over a concentration range of 60 - 8000 µg L-1 with low limits of detection in the range of 20 - 40 µg L-1. MCM-41-SPMTE required only minute amounts of adsorbent (3 mg) and desorption solvent (100 µL) and proved a successful extraction technique with high relative recoveries in the range of 82.5 - 111.0% for the analytes. MCM-41 was also employed as adsorbent in dispersive micro-solid phase extraction (D-µ-SPE) of six azole antifungal drugs including VRZ, KTZ, miconazole (MCZ), clotrimazole (CTZ), fluconazole (FLZ) and econazole (ECZ). The optimized D-µ- SPE was successfully applied to the determination of azole drugs in urine and human plasma. The method showed good linearity (r2 = 0.9900) over a concentration range of 0.1 - 10000 µg L-1, excellent limits of detection in the range of 0.001 - 1.500 µg L-1 and good relative recoveries in the range of 80.9 - 116.8%. A D-µ-SPE method incorporating new mesoporous carbon COU-2 as adsorbent was developed for the determination of three penicillins in water and milk samples. Under the optimized conditions, COU-2-D-µ-SPE showed excellent limits of detection in the range of 0.06 - 3.3 µg L-1 for oxacillin, cloxacillin and dicloxacillin with good linearity (r2 = 0.9992) in the concentration range of 0.1 - 5000 µg L-1 and good relative recoveries (80.3 - 113.6%). COU-2-D-µ-SPE is beneficial in terms of solvent saving, simplified analytical procedure and rapid extraction. The surface of COU-2 was further modified by functionalization with vinyl group to improve the extraction of target azole antifungal drugs by increasing the hydrophobicity of the adsorbent. Vinyl-COU-2 was used as adsorbent in D-µ-SPE (Vinyl-COU-2-D-µ-SPE) for the determination of azole antifungal drugs in water and biological samples. Excellent limits of detection (0.4 - 1.6 µg L-1) were obtained for KTZ and ITZ, respectively, with good linearity (r2 = 0.9959) in the concentration range of 1 - 400 µg L-1. The method provided high enrichment factors up to 92 with excellent relative recoveries in the range of 89.8 - 113.9% for both analytes. The developed microextraction techniques combined with liquid chromatography have proved to be simple, rapid and efficient with performances that are superior to those of conventional methods and suitable for the determination of azole drugs and penicillins in water, milk and biological samples. 2014-06 Thesis http://eprints.utm.my/id/eprint/78300/ http://eprints.utm.my/id/eprint/78300/1/NoorfatimahYahayaPFS2014.pdf application/pdf en public http://dms.library.utm.my:8080/vital/access/manager/Repository/vital:98003 phd doctoral Universiti Teknologi Malaysia, Faculty of Science Faculty of Science
institution	Universiti Teknologi Malaysia
collection	UTM Institutional Repository
language	English
topic	QD Chemistry
spellingShingle	QD Chemistry Yahaya, Noorfatimah New micro-solid phase extraction techniques based on mesoporous materials for selected antibiotic and antifungal agents
description	New microextraction techniques have been developed for sample preparation of azole drugs and penicillins in water, milk and biological samples prior to their liquid chromatographic determination. A microextraction method based on solid phase membrane tip extraction (SPMTE) incorporated with mesoporous silica, MCM-41, was developed for the determination of azole antifungal drugs, namely voriconazole (VRZ), ketoconazole (KTZ) and itraconazole (ITZ) in human plasma. Under the optimized conditions, the method demonstrated good linearity (r2 = 0.9958) over a concentration range of 60 - 8000 µg L-1 with low limits of detection in the range of 20 - 40 µg L-1. MCM-41-SPMTE required only minute amounts of adsorbent (3 mg) and desorption solvent (100 µL) and proved a successful extraction technique with high relative recoveries in the range of 82.5 - 111.0% for the analytes. MCM-41 was also employed as adsorbent in dispersive micro-solid phase extraction (D-µ-SPE) of six azole antifungal drugs including VRZ, KTZ, miconazole (MCZ), clotrimazole (CTZ), fluconazole (FLZ) and econazole (ECZ). The optimized D-µ- SPE was successfully applied to the determination of azole drugs in urine and human plasma. The method showed good linearity (r2 = 0.9900) over a concentration range of 0.1 - 10000 µg L-1, excellent limits of detection in the range of 0.001 - 1.500 µg L-1 and good relative recoveries in the range of 80.9 - 116.8%. A D-µ-SPE method incorporating new mesoporous carbon COU-2 as adsorbent was developed for the determination of three penicillins in water and milk samples. Under the optimized conditions, COU-2-D-µ-SPE showed excellent limits of detection in the range of 0.06 - 3.3 µg L-1 for oxacillin, cloxacillin and dicloxacillin with good linearity (r2 = 0.9992) in the concentration range of 0.1 - 5000 µg L-1 and good relative recoveries (80.3 - 113.6%). COU-2-D-µ-SPE is beneficial in terms of solvent saving, simplified analytical procedure and rapid extraction. The surface of COU-2 was further modified by functionalization with vinyl group to improve the extraction of target azole antifungal drugs by increasing the hydrophobicity of the adsorbent. Vinyl-COU-2 was used as adsorbent in D-µ-SPE (Vinyl-COU-2-D-µ-SPE) for the determination of azole antifungal drugs in water and biological samples. Excellent limits of detection (0.4 - 1.6 µg L-1) were obtained for KTZ and ITZ, respectively, with good linearity (r2 = 0.9959) in the concentration range of 1 - 400 µg L-1. The method provided high enrichment factors up to 92 with excellent relative recoveries in the range of 89.8 - 113.9% for both analytes. The developed microextraction techniques combined with liquid chromatography have proved to be simple, rapid and efficient with performances that are superior to those of conventional methods and suitable for the determination of azole drugs and penicillins in water, milk and biological samples.
format	Thesis
qualification_name	Doctor of Philosophy (PhD.)
qualification_level	Doctorate
author	Yahaya, Noorfatimah
author_facet	Yahaya, Noorfatimah
author_sort	Yahaya, Noorfatimah
title	New micro-solid phase extraction techniques based on mesoporous materials for selected antibiotic and antifungal agents
title_short	New micro-solid phase extraction techniques based on mesoporous materials for selected antibiotic and antifungal agents
title_full	New micro-solid phase extraction techniques based on mesoporous materials for selected antibiotic and antifungal agents
title_fullStr	New micro-solid phase extraction techniques based on mesoporous materials for selected antibiotic and antifungal agents
title_full_unstemmed	New micro-solid phase extraction techniques based on mesoporous materials for selected antibiotic and antifungal agents
title_sort	new micro-solid phase extraction techniques based on mesoporous materials for selected antibiotic and antifungal agents
granting_institution	Universiti Teknologi Malaysia, Faculty of Science
granting_department	Faculty of Science
publishDate	2014
url	http://eprints.utm.my/id/eprint/78300/1/NoorfatimahYahayaPFS2014.pdf
_version_	1747817955572318208

New micro-solid phase extraction techniques based on mesoporous materials for selected antibiotic and antifungal agents

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