Method development for the determination of sulphonamide residues in chicken by liquid chromatography ion trap tandem mass spectrometry
| dc.contributor.author | Ahmad, Sidek | |
| dc.date.accessioned | 2014-11-04T02:54:59Z | |
| dc.date.available | 2014-11-04T02:54:59Z | |
| dc.date.issued | 2006 | |
| dc.description | Master | en_US |
| dc.description.abstract | A simple, sensitive and reliable method for the determination of five sulphonamide residues (sulphadiazine, sulphamethazine, sulphaquinoxaline and sulphadimethoxine) in chicken was developed using a combination of high performance liquid chromatography (HPLC) with ion trap tandem mass spectrometry. Sample extraction involvd extraction with acetonitrile, removal of fat with n-hexane followed by purification of the extract with Strata X polymeric sorbent Solid Phase Eextraction cartridge after reconstitution with 0.2 M phosphoric acid. The extract was eluted with methanol and evaporated to dryness in a water bath under constant flow of nitrogen gas. The residue was again reconstituted with a solution mixture of 0.1 % acetic acid in ultra pure water and acetonitrile (1:1). A liquid chromatograph with an electrospray ionization interface to the ion trap tandem mass spectrometrer (LC-MS-MS) was used for simultaneous confirmation and quantitation of the sulphonamide residues. A narrow bore HPLC column, Genesis C18 120 (Å, 3 m, 5 cm x 2.1 mm) and a solution of 0.1 % acetic acid in ultra pure water and acetonitrile (65:35) with a flow rate 60 μl/min was used to separate the sulphonamides. The analytical procedure for the detection of sulphonamide residues was validated and the measurement of uncertainty was determined for the compliance of the ISO/IEC 17025 quality system requirement. During validation, specificity, linearity, limit of detection (LOD), limit of quantitation (LOQ), precision and accuracy of the method was determined. New product ions that could be used for confirmation and quantitation at m/z 174 for sulphadiazine, sulphamethazine and sulphaquinoxaline, at m/z 204 for sulphamethazine and m/z 226 for sulphaquinoxaline were observed. A linear plot was obtained for a concentration range between 20 ppb and 400 ppb for sulphadiazine, sulphaquinoxaline and sulphadimethoxine and 10 ppb to 400 ppb for sulphamethazin, respectively, where the regression coefficient for each calibration range obtained was 0.999. The limit of detection (LOD) was 2 ppb for sulphamethazine and 5 ppb for sulphadiazine, sulphaquinoxaline and sulphadimethoxine, respectively. The limit of quantification (LOQ) was 10ppb for sulphamethazine and 20 ppb for sulphadiazine, sulphaquinoxaline and sulphadimethoxine, respectively. The extraction recovery for spiked samples at the LOQ level was 51, 54, 68 and 83 % with coefficient of variation of 5, 13, 9, and 7 % for sulphadiazine, sulphamethazine, sulphaquinoxaline and sulphadimethoxine, respectively and the expanded uncertainty values at concentration of 100 ppb for sulphadiazine, sulphamethazine, sulphaquinoxaline and sulphadimethoxine were 6, 9, 10 and 4 ppb, respectively. Therefore from the performance characteristic obtained the developed method could be reliably used for routine analytical work. | en_US |
| dc.identifier.uri | http://hdl.handle.net/123456789/369 | |
| dc.language.iso | en | en_US |
| dc.subject | Chemical science | en_US |
| dc.subject | Sulphonamide residues | en_US |
| dc.subject | Chromatography ion | en_US |
| dc.title | Method development for the determination of sulphonamide residues in chicken by liquid chromatography ion trap tandem mass spectrometry | en_US |
| dc.type | Thesis | en_US |
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