@article {654, title = {Isolation, Method Development, and Validation of Diterpenes in Coffee Oil: Identification by Multiple Reaction Monitoring Approach with Atmospheric Pressure Chemical Ionization Mode}, journal = {Pharmacognosy Research}, volume = {13}, year = {2021}, month = {April 2021}, pages = {42-48}, type = {Original Article}, chapter = {42}, abstract = {

Objectives:\ The aim of the present study is to isolation, identification, and quantification of free diterpenes in coffee oil of\ Coffea arabica.\ Materials and Methods:\ For the isolation of free diterpenes, saponification reaction step was employed and followed with a liquid-liquid extraction procedure applied. Cafestol and kahweol were identified by multiple reaction monitoring (MRM) of positive ionization (MRM) mode of atmospheric pressure chemical ionization (APCI) mass spectrometry detection. The quantification of free diterpenes was done by high-performance liquid chromatography with diode array detector. The developed method was validated according to the international conference on harmonization guidelines.\ Results:\ The ion transitions of the precursor to the product ion at (M + H)+m/z\ 317.20{\textrightarrow}146.90, 281.00, 299.00 for cafestol and 315.10{\textrightarrow}144.90, 278.90, 296.90 for kahweol were observed. The proposed method was validated for linearity with excellent correlation coefficient of cafestol and kahweol were found to be 0.9997 and 0.9996, respectively. The intra-day and intermediate precisions and repeatability showed the percentage relative standard deviation was \<1\%. The recovery rate for cafestol and kahweol were observed to be in the acceptable limit of 95.303\%{\textendash}98.539\% and 95.963\%{\textendash}97.174\%, respectively. The limit of detection of cafestol and kahweol were found to be 6.81 and 7.35 ppm, respectively. The limit of quantitation (LOQ) was found to be 22.72 and 24.52 ppm, respectively.\ Conclusion:\ The developed method is simple, rapid, precise, accurate and it is recommended for efficient assays in routine work.

}, keywords = {Atmospheric pressure chemical ionization, Cafestol, Coffea arabica, Kahweol, Method validation}, doi = {10.4103/pr.pr_66_20}, author = {Naveen Puttaswamy and Lingaraju Harakanahalli Basavegowda and Deepak Machettira and Chandrappa Siddappa and Rashmi Ramesh and Shyam Prasad Kodimule} } @article {93, title = {Development and Validation of Veratric Acid in Tabebuia avellanedae using Liquid Chromatography-Electrospray Ionization-Mass Spectrometry/Mass Spectrometry-Multiple Reaction Monitoring-Based Assay Coupled with 1,1-Diphenyl-2-Picrylhydrazyl Method}, journal = {Pharmacognosy Research}, volume = {12}, year = {2020}, month = {May 2020}, pages = {107-111}, type = {Original Article}, chapter = {107}, abstract = {

Objective: The aim of the present study is to develop a new simple, precise, and accurate liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantification of veratric acid in Tabebuia avellanedae Linn. Materials and Methods: The quantification of veratric acid was done using collision-induced dissociation multiple reaction monitoring scan of mass spectrometry technique. The developed method was validated according to the International Conference on Harmonization guidelines. The free radical scavenging activity was performed by 1,1-diphenyl-2-picrylhydrazyl (DPPH) method. Results: The ion transitions of the precursor to the productions were principally protonated ion [M + H]+ at m/z 182.8 \>139.20, 124.20, and 77.0 for veratric acid. The proposed method was validated for linearity with an excellent correlation coefficient of 0.9978. The intraday and intermediate precisions and repeatability showed the percentage relative standard deviation was \<2\%. The accuracy for the determination of veratric acid was within 82.20\%{\textendash}97.65\%. The limit of detection and limit of quantitation were 0.66 and 2.21 ppm, respectively. The half-maximal inhibitory concentration value for the DPPH radical scavenging activity of ascorbic acid and quality control sample (hydroalcoholic extract of T. avellanedae) was found to be 17.79 and 36.44 μg/ml, respectively. Conclusion: The developed LC-MS/MS method is a simple, rapid, precise, accurate, and it is recommended for efficient assays in routine work. T. avellanedae exhibited strong DPPH radical scavenging activity.

}, keywords = {1, 1-diphenyl-2-picrylhydrazyl, Method validation, Multiple reaction monitoring, Tabebuia avellanedae, Veratric acid}, doi = {10.4103/pr.pr_77_19}, author = {Puttaswamy Naveen and Harakanahalli Basavegowda Lingaraju and Siddappa Chandrappa and Srikant Anitha and Kodimule Shyam Prasad} }