Novel Strategies using Micro Pressurized Liquid Extraction to Rapidly Prepare Solid Samples for Analysis

This thesis will describe several advancements in solid-liquid extraction methods using new applications of a micro preparative technique. The overall aim is to reduce solvent consumption and analysis times to promote quick, low solvent approaches to solid sample preparation. Additionally, this technique will be shown to integrate directly with chromatographic instruments to promote a hands-free analysis approach. In particular, the first portion of this thesis explores a novel on-line micro pressurized liquid extraction method that directly interfaces solid sample preparation with high performance liquid chromatography. The technique employs rapid heating to remove analytes from milligram quantities of sample in as little as 20-40 seconds. As applications, the system was applied to a variety of solid samples including pharmaceutical tablets, green tea leaves, and samples containing polycyclic aromatic hydrocarbons. This micro preparative approach will be shown to provide rapid, quantitative extractions when compared to conventional methods. Frequently, total analysis times for a given sample can be as quick as 95 seconds which represents a large improvement over techniques such as Soxhlet or conventional pressurized liquid extraction. Next, a method that combines on-line micro pressurized liquid extraction with solid phase trapping will be introduced. Rapid heating will be again employed to extract analytes of interest from milligram quantities of solid samples before internally transferring this extract to a solid phase trap. Analyte will be shown to effectively absorb and concentrate on this solid phase material before it is subsequently desorbed/injected to high performance liquid chromatography for analysis. As a result, samples with low level analytes will be shown to have greatly improved detection limits which facilitates their characterization and analysis. Several applications of this method will be presented, and the results will indicate that on-line micro pressurized liquid extraction – solid phase extraction can facilitate coupling to high performance liquid chromatography and provide rapid sample preparation using little solvent.

Name thesis:degree_name

Master of Science (MSc)

Discipline thesis:degree_discipline

Chemistry

Grantor dc:publisher.institution

Science

Year dc:date.issued

2020

Author dc:creator

• Taylor, Bradley Mark

Advisor dc:contributor.advisor

• Thurbide, Kevin B.

Committee members dc:contributor.committeemember

• Heyne, Belinda
• Marriott, Robert A.

Statement dc:rights

• University of Calgary graduate students retain copyright ownership and moral rights for their thesis. You may use this material in any way that is permitted by the Copyright Act or through licensing that has been assigned to the document. For uses that are not allowable under copyright legislation or licensing, you are required to seek permission.

Language dc:language.iso

eng

DOI

http://dx.doi.org/10.11575/PRISM/38342

OAI identifier oai:identifier

oai:ucalgary.scholaris.ca:1880/112699