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Optimal analysis of sulfonamides fro...

Combs, Michael Terry.

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Optimal analysis of sulfonamides from biological matrices using supercritical fluids.

Record Type:	Electronic resources : Monograph/item
Title/Author:	Optimal analysis of sulfonamides from biological matrices using supercritical fluids./
Author:	Combs, Michael Terry.
Published:	Ann Arbor : ProQuest Dissertations & Theses, : 1997,
Description:	119 p.
Notes:	Source: Dissertation Abstracts International, Volume: 59-12, Section: B, page: 6296.
Contained By:	Dissertation Abstracts International59-12B.
Subject:	Analytical chemistry. -
Online resource:	http://pqdd.sinica.edu.tw/twdaoapp/servlet/advanced?query=9914706
ISBN:	9780599133358

Optimal analysis of sulfonamides from biological matrices using supercritical fluids.
Combs, Michael Terry.

Optimal analysis of sulfonamides from biological matrices using supercritical fluids. - Ann Arbor : ProQuest Dissertations & Theses, 1997 - 119 p.

Source: Dissertation Abstracts International, Volume: 59-12, Section: B, page: 6296.

Thesis (Ph.D.)--Virginia Polytechnic Institute and State University, 1997.

The objective of this research was to develop new sample preparation procedures for the isolation of sulfonamides, as well as, to determine the applicability of employing on-line nitrogen selective and mass spectrometric detection methods.

ISBN: 9780599133358Subjects--Topical Terms:

3168300
Analytical chemistry.

Optimal analysis of sulfonamides from biological matrices using supercritical fluids.
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020 $a 9780599133358
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100 1 $a Combs, Michael Terry. $3 3278715
245 1 0 $a Optimal analysis of sulfonamides from biological matrices using supercritical fluids.
260 1 $a Ann Arbor : $b ProQuest Dissertations & Theses, $c 1997
300 $a 119 p.
500 $a Source: Dissertation Abstracts International, Volume: 59-12, Section: B, page: 6296.
500 $a Chair: Larry T. Taylor.
502 $a Thesis (Ph.D.)--Virginia Polytechnic Institute and State University, 1997.
520 $a The objective of this research was to develop new sample preparation procedures for the isolation of sulfonamides, as well as, to determine the applicability of employing on-line nitrogen selective and mass spectrometric detection methods.
520 $a The first phase of this research investigated the effect of temperature and pressure on the supercritical fluid extraction (SFE) of sulfonamides from a spiked sand matrix. Temperature effects were either positive or negative with respect to extraction rate and total recovery, depending on the pressure and extraction fluid employed.
520 $a The second portion of this research compared trifluoromethane (CHF 3) and carbon dioxide (CO2) as fluids for the extraction of sulfonamides from spiked non-fat dry milk, beef liver, and egg yolk were found to be more selective using CHF3 than CO2. The polar trifluoromethane improved the extraction efficiency of the polar sulfonamides from the biological matrices and also reduced the amount of co-extractives.
520 $a The next phase of this research considered the effect of organic modifier and CO2 in the SFE of sulfonamides from chicken liver, beef liver and egg yolk. Methanol, ethanol, acetone, acetonitrile were compared to determine optimum conditions. A SFE method employing 20% acetonitrile modified CO 2 yielded quantitative recovery of sulfonamides from chicken liver, but 20% acetone modified CO2 was required to obtain quantitative recovery from beef liver. Either 20% acetone or 20% acetonitrile yielded quantitative recovery from egg yolk.
520 $a The last phase of this research focused on the evaluation of selective detection methods for sulfonamide analysis. Chemiluminescence nitrogen detection (CLND) parameters were optimized for use with packed column supercritical fluid chromatography (SFQ yielding a minimum detectable quantity (MDQ) of 5 ng of sulfamethazine, on column. Improvements in the detector design decreased the MDQ to 0.5 ng, while, decreasing the column diameter further reduced the MDQ to 125 pg. The second part of this phase evaluated HPLC/Atmospheric pressure chemical ionization (APCI) mass spectrometry for the detection of sulfonamides. Sensitivity in selective ion mode was found to be as low as 50 pg on column for sulfamethazine. Supercritical fluid extracts of sulfonamides spiked at 100mug/kg in chicken liver were found to be readily detected by this method.
590 $a School code: 0247.
650 4 $a Analytical chemistry. $3 3168300
650 4 $a Food science. $3 3173303
690 $a 0486
690 $a 0359
710 2 $a Virginia Polytechnic Institute and State University. $3 1017496
773 0 $t Dissertation Abstracts International $g 59-12B.
790 $a 0247
791 $a Ph.D.
792 $a 1997
793 $a English
856 4 0 $u http://pqdd.sinica.edu.tw/twdaoapp/servlet/advanced?query=9914706