Ultrasound-assisted low-density solvent dispersive liquid–liquid microextraction for the determination of 4 designer benzodiazepines in urine samples by gas chromatography–triple quadrupole mass spectrometry

Meng, L; Zhu, B; Zheng, K; Fu, S

Ultrasound-assisted low-density solvent dispersive liquid–liquid microextraction for the determination of 4 designer benzodiazepines in urine samples by gas chromatography–triple quadrupole mass spectrometry

Meng, L Zhu, B Zheng, K Fu, S

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Publication Type:: Journal Article
Citation:: Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences, 2017, 1053 pp. 9 - 15
Issue Date:: 2017-05-15

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Field	Value	Language
dc.contributor.author	Meng, L	en_US
dc.contributor.author	Zhu, B	en_US
dc.contributor.author	Zheng, K	en_US
dc.contributor.author	Fu, S https://orcid.org/0000-0002-6238-3612	en_US
dc.date.available	2017-04-02	en_US
dc.date.issued	2017-05-15	en_US
dc.identifier.citation	Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences, 2017, 1053 pp. 9 - 15	en_US
dc.identifier.issn	1570-0232	en_US
dc.identifier.uri	http://hdl.handle.net/10453/124294
dc.description.abstract	© 2017 Elsevier B.V. A novel microextraction technique based on ultrasound-assisted low-density solvent dispersive liquid–liquid microextraction (UA-LDS-DLLME) had been applied for the determination of 4 designer benzodiazepines (phenazepam, diclazepam, flubromazepam and etizolam) in urine samples by gas chromatography- triple quadrupole mass spectrometry (GC-QQQ-MS). Ethyl acetate (168 μL) was added into the urine samples after adjusting pH to 11.3. The samples were sonicated in an ultrasonic bath for 5.5 min to form a cloudy suspension. After centrifugation at 10000 rpm for 3 min, the supernatant extractant was withdrawn and injected into the GC-QQQ-MS for analysis. Parameters affecting the extraction efficiency have been investigated and optimized by means of single factor experiment and response surface methodology (Box-Behnken design). Under the optimum extraction conditions, a recovery of 73.8–85.5% were obtained for all analytes. The analytical method was linear for all analytes in the range from 0.003 to 10 μg/mL with the correlation coefficient ranging from 0.9978 to 0.9990. The LODs were estimated to be 1–3 ng/mL. The accuracy (expressed as mean relative error MRE) was within ±5.8% and the precision (expressed as relative standard error RSD) was less than 5.9%. UA-LDS-DLLME technique has the advantages of shorter extraction time and is suitable for simultaneous pretreatment of samples in batches. The combination of UA-LDS-DLLME with GC–QQQ–MS offers an alternative analytical approach for the sensitive detection of these designer benzodiazepines in urine matrix for clinical and medico-legal purposes.	en_US
dc.relation.ispartof	Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences	en_US
dc.relation.isbasedon	10.1016/j.jchromb.2017.04.008	en_US
dc.subject.mesh	Humans	en_US
dc.subject.mesh	Benzodiazepines	en_US
dc.subject.mesh	Diazepam	en_US
dc.subject.mesh	Central Nervous System Agents	en_US
dc.subject.mesh	Designer Drugs	en_US
dc.subject.mesh	Substance Abuse Detection	en_US
dc.subject.mesh	Sonication	en_US
dc.subject.mesh	Gas Chromatography-Mass Spectrometry	en_US
dc.subject.mesh	Limit of Detection	en_US
dc.subject.mesh	Liquid Phase Microextraction	en_US
dc.title	Ultrasound-assisted low-density solvent dispersive liquid–liquid microextraction for the determination of 4 designer benzodiazepines in urine samples by gas chromatography–triple quadrupole mass spectrometry	en_US
dc.type	Journal Article
utslib.citation.volume	1053	en_US
utslib.for	0301 Analytical Chemistry	en_US
utslib.for	0601 Biochemistry and Cell Biology	en_US
utslib.for	1115 Pharmacology and Pharmaceutical Sciences	en_US
pubs.embargo.period	Not known	en_US
pubs.organisational-group	/University of Technology Sydney
pubs.organisational-group	/University of Technology Sydney/Faculty of Science
pubs.organisational-group	/University of Technology Sydney/Faculty of Science/School of Mathematical and Physical Sciences
pubs.organisational-group	/University of Technology Sydney/Strength - CCET - Centre for Clean Energy Technology
pubs.organisational-group	/University of Technology Sydney/Strength - CFS - Centre for Forensic Science
utslib.copyright.status	closed_access
pubs.publication-status	Published	en_US
pubs.volume	1053	en_US

Abstract:

© 2017 Elsevier B.V. A novel microextraction technique based on ultrasound-assisted low-density solvent dispersive liquid–liquid microextraction (UA-LDS-DLLME) had been applied for the determination of 4 designer benzodiazepines (phenazepam, diclazepam, flubromazepam and etizolam) in urine samples by gas chromatography- triple quadrupole mass spectrometry (GC-QQQ-MS). Ethyl acetate (168 μL) was added into the urine samples after adjusting pH to 11.3. The samples were sonicated in an ultrasonic bath for 5.5 min to form a cloudy suspension. After centrifugation at 10000 rpm for 3 min, the supernatant extractant was withdrawn and injected into the GC-QQQ-MS for analysis. Parameters affecting the extraction efficiency have been investigated and optimized by means of single factor experiment and response surface methodology (Box-Behnken design). Under the optimum extraction conditions, a recovery of 73.8–85.5% were obtained for all analytes. The analytical method was linear for all analytes in the range from 0.003 to 10 μg/mL with the correlation coefficient ranging from 0.9978 to 0.9990. The LODs were estimated to be 1–3 ng/mL. The accuracy (expressed as mean relative error MRE) was within ±5.8% and the precision (expressed as relative standard error RSD) was less than 5.9%. UA-LDS-DLLME technique has the advantages of shorter extraction time and is suitable for simultaneous pretreatment of samples in batches. The combination of UA-LDS-DLLME with GC–QQQ–MS offers an alternative analytical approach for the sensitive detection of these designer benzodiazepines in urine matrix for clinical and medico-legal purposes.

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http://hdl.handle.net/10453/124294