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Quantitative Determination of Solanesol in Tobacco by Liquid Chromatography–Mass Spectrometry (LC-MS)


Affiliations
1 Bio-Pharma Laboratories Pvt.Ltd., Guntur-522002, Andhra Pradesh, India
2 Department of Organic Chemistry, Andhra University, Visakhapatnam-530003, A. P., India
3 Division of Crop Chemistry and Soil Science, Central Tobacco Research Institute, Rajahmundry-533105, Andhra Pradesh, India
4 Department of Chemistry, Acharya Nagarjuna University, Nagarjuna Nagar-522510, A. P., India
     

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A rapid and sensitive liquid chromatography-mass spectrometry (LC-MS/MS) method with multiple reaction monitoring (MRM) was developed for the determination of solanesol in tobacco. Sample preparation was performed by ultrasonic extraction with methanol and then supernatant was extracted with hexane. The method used atmospheric pressure chemical ionization (APCI) detection in positive-ion mode. The separation of solanesol was performed on a Symmetry RP18 column with a mixture of acetonitrile and isopropanol (1:1, v/v) containing 2mM ammonium acetate as mobile phase. Quantification of solanesol was performed by the standard addition method. The limit of quantification (LOQ) and limit of detection (LOD) of solanesol were, respectively, 5.0 ng/ml (S/N = 10) and 1.5 ng/ml (S/N = 3). The relative standard deviations of peak area were 0.89 and 1.12% for intra-day and inter-day, respectively. The recovery of solanesol ranged from 97.72 to 99.67% and the corresponding R.S.D.s were less than 2.7%. Analysis took 5 min, making the method suitable for rapid determination of solanesol in tobacco. The proposed method has been successfully applied to the analysis of solanesol in various tobacco samples.


Keywords

LC–MS/MS, MRM, APCI, Tobacco, Solanesol.
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  • Quantitative Determination of Solanesol in Tobacco by Liquid Chromatography–Mass Spectrometry (LC-MS)

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Authors

K. Mahendra
Bio-Pharma Laboratories Pvt.Ltd., Guntur-522002, Andhra Pradesh, India
Y. L. N. Murthy
Department of Organic Chemistry, Andhra University, Visakhapatnam-530003, A. P., India
C. V. Narasimha Rao
Division of Crop Chemistry and Soil Science, Central Tobacco Research Institute, Rajahmundry-533105, Andhra Pradesh, India
K. Bala Murali Krishna
Department of Chemistry, Acharya Nagarjuna University, Nagarjuna Nagar-522510, A. P., India

Abstract


A rapid and sensitive liquid chromatography-mass spectrometry (LC-MS/MS) method with multiple reaction monitoring (MRM) was developed for the determination of solanesol in tobacco. Sample preparation was performed by ultrasonic extraction with methanol and then supernatant was extracted with hexane. The method used atmospheric pressure chemical ionization (APCI) detection in positive-ion mode. The separation of solanesol was performed on a Symmetry RP18 column with a mixture of acetonitrile and isopropanol (1:1, v/v) containing 2mM ammonium acetate as mobile phase. Quantification of solanesol was performed by the standard addition method. The limit of quantification (LOQ) and limit of detection (LOD) of solanesol were, respectively, 5.0 ng/ml (S/N = 10) and 1.5 ng/ml (S/N = 3). The relative standard deviations of peak area were 0.89 and 1.12% for intra-day and inter-day, respectively. The recovery of solanesol ranged from 97.72 to 99.67% and the corresponding R.S.D.s were less than 2.7%. Analysis took 5 min, making the method suitable for rapid determination of solanesol in tobacco. The proposed method has been successfully applied to the analysis of solanesol in various tobacco samples.


Keywords


LC–MS/MS, MRM, APCI, Tobacco, Solanesol.