@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 {230, title = {Method Development and Validation for the Determination of Caffeine: An Alkaloid from Coffea arabica by High-performance Liquid Chromatography Method}, journal = {Pharmacognosy Research}, volume = {10}, year = {2018}, month = {February 2018}, pages = {88-91}, type = {Original Article}, chapter = {88}, abstract = {

Objective: The present study was investigated to develop and validate a reversed phase high performance liquid chromatography method for the determination of caffeine from bean material of Coffee arabica. Materials and Methods: The separation was achieved on a reversedphase C18 column using a mobile phase composed of water: methanol (50:50) at a flow rate of 1.0 mlmin-1. The detection was carried out on a UV detector at 272 nm. The developed method was validated according to the requirements for International Conference on Harmonisation (ICH) guidelines, which includes specificity, linearity, precision, accuracy, limit of detection and limit of quantitation. Results: The developed method validates good linearity with excellent correlation coefficient (R2 \> 0.999). In repeatability and intermediate precision, the percentage relative standard deviation (\% RSD) of peak area was less than 1\% shows high precision of the method. The recovery rate for caffeine was within 98.78\% - 101.28\% indicates high accuracy of the method. The low limit of detection and limit of quantitation of caffeine enable the detection and quantitation of caffeine from C. arabica at low concentrations. Conclusion: The developed HPLC method is a simple, rapid, precisely, accurately and widely accepted and it is recommended for efficient assays in routine work.

}, keywords = {Caffeine, Coffea arabica, Linearity, Precision, Recovery}, doi = {10.4103/pr.pr_79_17}, author = {P Naveen and HB Lingaraju and M Deepak and B Medhini and K Shyam Prasad} }