Simultaneous quantification of idelalisib, fludarabine and lenalidomide in rat plasma by using high-performance liquid chromatography coupled with heated electrospray ionization tandem mass spectrometry.
A sensitive and reliable high-performance liquid chromatography-mass spectrometry (LC-MS/MS) method was developed and validated for simultaneous quantification of idelalisib, fludarabine and lenalidomide using tolbutamide as an internal standard. Analytes were recovered by liquid-liquid extraction and separated on a reverse phase C18 column (150mm×4.6mm i.d., 5μm) using methanol:0.1% formic acid buffer (70:30) as mobile phase at a flow rate of 1mL/min in isocratic mode. Selective reaction monitoring was performed using the transitions, i.e. m/z 416.25/176.48, 286.11/154.10, 260.15/149.15, and 271.14/155.06 to quantify idelalisib, fludarabine and lenalidomide and tolbutamide, respectively. The method was validated over the concentration range of 1.15-576.84ng/mL for idelalisib, 0.95-476.25ng/mL for fludarabine and 0.97-486.19ng/mL for lenalidomide. Intra and inter-day accuracy and precision of validated method were within the acceptable limits of <15%. Coefficients of correlation (r(2)) for the calibration curves were >0.998 for all analytes. The method was successfully applied for simultaneous estimation of idelalisib, fludarabine and lenalidomide in a pharmacokinetic study in rats.
Incozen Therapeutics Private Limited, 450, Alexandira Knowledge Park, Turkapplly, Hyderabad 500078, Andhra Pradesh, India; CRD, PRIST University, Vallam, Thanjavur 613403. Tamilnadu, India. Electronic address: sridharveeraraghavan@gmail.com.
Sridhar
S
Veeraraghavan
Incozen Therapeutics Private Limited, 450, Alexandira Knowledge Park, Turkapplly, Hyderabad 500078, Andhra Pradesh, India.
Satheeshmanikandan
S
Thappali
Incozen Therapeutics Private Limited, 450, Alexandira Knowledge Park, Turkapplly, Hyderabad 500078, Andhra Pradesh, India.
Srikant
S
Viswanadha
Incozen Therapeutics Private Limited, 450, Alexandira Knowledge Park, Turkapplly, Hyderabad 500078, Andhra Pradesh, India.
Santhoshkumar
S
Nalla
Incozen Therapeutics Private Limited, 450, Alexandira Knowledge Park, Turkapplly, Hyderabad 500078, Andhra Pradesh, India.
Sandhyarani
S
Chennupati
Incozen Therapeutics Private Limited, 450, Alexandira Knowledge Park, Turkapplly, Hyderabad 500078, Andhra Pradesh, India.
Manikantakumar
M
Golla
Incozen Therapeutics Private Limited, 450, Alexandira Knowledge Park, Turkapplly, Hyderabad 500078, Andhra Pradesh, India.
Swaroopkumar
S
Vakkalanka
Dept of Pharmaceutics, Annai JKK Sampoorani Ammal College of Pharmacy, Komarapalayam, Namakkal, 638 183, Tamilnadu, India.
Manivannan
M
Rangasamy
D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004355:Drug Stability; D000077269:Lenalidomide; D008297:Male; D011687:Purines / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics; D052999:Quinazolinones / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics; D051381:Rats; D017208:Rats, Wistar; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods; D013792:Thalidomide / Q000031:analogs & derivatives* / Q000097:blood / Q000737:chemistry / Q000493:pharmacokinetics; D014740:Vidarabine / Q000031:analogs & derivatives* / Q000097:blood / Q000737:chemistry / Q000493:pharmacokinetics
D011687:Purines; D052999:Quinazolinones; D013792:Thalidomide; D000077269:Lenalidomide; D014740:Vidarabine; C024352:fludarabine; C552946:idelalisib
Bioanalytical; Fludarabine; Idelalisib; LC-MS/MS; Lenalidomide; Pharmacokinetics