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Determination of cyclamate in urine by derivatized gas chromatography-mass spectrometry

AIM: It is important in toxicological/drug screening work to rule out the possible interfering analytes, to eliminate the false positive or negative results. In this paper, we describe a simple, selective, and sensitive derivatized GC-MS method for the determination of cyclohexylsulfamic acid (cycla...

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Autores principales: Idris, Mohd, Middha, Deepak, Rasool, Shaik N., Shukla, Sudhir K., Baggi, Tulsidas R.
Formato: Online Artículo Texto
Lenguaje:English
Publicado: Medknow Publications & Media Pvt Ltd 2013
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3612338/
https://www.ncbi.nlm.nih.gov/pubmed/23559823
http://dx.doi.org/10.4103/0975-7406.106566
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author Idris, Mohd
Middha, Deepak
Rasool, Shaik N.
Shukla, Sudhir K.
Baggi, Tulsidas R.
author_facet Idris, Mohd
Middha, Deepak
Rasool, Shaik N.
Shukla, Sudhir K.
Baggi, Tulsidas R.
author_sort Idris, Mohd
collection PubMed
description AIM: It is important in toxicological/drug screening work to rule out the possible interfering analytes, to eliminate the false positive or negative results. In this paper, we describe a simple, selective, and sensitive derivatized GC-MS method for the determination of cyclohexylsulfamic acid (cyclamate) in urine. MATERIALS AND METHODS: Elite- 5MS capillary column was used for the separation of analytes and detection using GC-MS. The analysis was carried out in selected ion monitoring mode (SIM) in the range of 26 to 200 using m/z values of 57, 30, 55, 41, 44, 67, 82, 98, and 39. RESULTS AND DISCUSSION: The method is based on the conversion of cyclamate into nitroso derivative of cyclamate followed by its gas chromatography-mass spectrometry determination. The limit of detection, limit of quantitation, and linearity range of the proposed method were found to be 0.2 μg/ ml, 0.7 μg/ml, and 1-15 μg/ml, respectively. The recovery of the present method is in the range of 88-94%. CONCLUSION: The proposed method can be applied for detection and quantification of cyclamate in urine.
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spelling pubmed-36123382013-04-04 Determination of cyclamate in urine by derivatized gas chromatography-mass spectrometry Idris, Mohd Middha, Deepak Rasool, Shaik N. Shukla, Sudhir K. Baggi, Tulsidas R. J Pharm Bioallied Sci Original Article AIM: It is important in toxicological/drug screening work to rule out the possible interfering analytes, to eliminate the false positive or negative results. In this paper, we describe a simple, selective, and sensitive derivatized GC-MS method for the determination of cyclohexylsulfamic acid (cyclamate) in urine. MATERIALS AND METHODS: Elite- 5MS capillary column was used for the separation of analytes and detection using GC-MS. The analysis was carried out in selected ion monitoring mode (SIM) in the range of 26 to 200 using m/z values of 57, 30, 55, 41, 44, 67, 82, 98, and 39. RESULTS AND DISCUSSION: The method is based on the conversion of cyclamate into nitroso derivative of cyclamate followed by its gas chromatography-mass spectrometry determination. The limit of detection, limit of quantitation, and linearity range of the proposed method were found to be 0.2 μg/ ml, 0.7 μg/ml, and 1-15 μg/ml, respectively. The recovery of the present method is in the range of 88-94%. CONCLUSION: The proposed method can be applied for detection and quantification of cyclamate in urine. Medknow Publications & Media Pvt Ltd 2013 /pmc/articles/PMC3612338/ /pubmed/23559823 http://dx.doi.org/10.4103/0975-7406.106566 Text en Copyright: © Journal of Pharmacy and Bioallied Sciences http://creativecommons.org/licenses/by-nc-sa/3.0 This is an open-access article distributed under the terms of the Creative Commons Attribution-Noncommercial-Share Alike 3.0 Unported, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
spellingShingle Original Article
Idris, Mohd
Middha, Deepak
Rasool, Shaik N.
Shukla, Sudhir K.
Baggi, Tulsidas R.
Determination of cyclamate in urine by derivatized gas chromatography-mass spectrometry
title Determination of cyclamate in urine by derivatized gas chromatography-mass spectrometry
title_full Determination of cyclamate in urine by derivatized gas chromatography-mass spectrometry
title_fullStr Determination of cyclamate in urine by derivatized gas chromatography-mass spectrometry
title_full_unstemmed Determination of cyclamate in urine by derivatized gas chromatography-mass spectrometry
title_short Determination of cyclamate in urine by derivatized gas chromatography-mass spectrometry
title_sort determination of cyclamate in urine by derivatized gas chromatography-mass spectrometry
topic Original Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3612338/
https://www.ncbi.nlm.nih.gov/pubmed/23559823
http://dx.doi.org/10.4103/0975-7406.106566
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