02736nas a2200253 4500008004100000245018600041210006900227260001500296300001000311490000700321520182800328653004502156653001302201653001902214653001202233653002202245100002302267700003902290700002302329700002502352700001902377700002802396856005802424 2021 eng d00aIsolation, Method Development, and Validation of Diterpenes in Coffee Oil: Identification by Multiple Reaction Monitoring Approach with Atmospheric Pressure Chemical Ionization Mode0 aIsolation Method Development and Validation of Diterpenes in Cof cApril 2021 a42-480 v133 a

Objectives: The aim of the present study is to isolation, identification, and quantification of free diterpenes in coffee oil of Coffea arabicaMaterials 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→146.90, 281.00, 299.00 for cafestol and 315.10→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%–98.539% and 95.963%–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.

10aAtmospheric pressure chemical ionization10aCafestol10aCoffea arabica10aKahweol10aMethod validation1 aPuttaswamy, Naveen1 aBasavegowda, Lingaraju, Harakanaha1 aMachettira, Deepak1 aSiddappa, Chandrappa1 aRamesh, Rashmi1 aKodimule, Shyam, Prasad uhttps://phcogres.com/article/2021/13/1/104103prpr6620