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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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Detalles Bibliográficos
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
Descripción
Sumario: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.