Determination of 10 pesticides, newly registered in Egypt, using modified QuEChERS method in combination with gas and liquid chromatography coupled with tandem mass spectrometric detection

Author(s):  
Mostafa Soliman ◽  
Mona A. Khorshid ◽  
Ashraf M. El-Marsafy ◽  
Mohamed M. Abo-Aly ◽  
Tawfeek Khedr
2020 ◽  
Vol 15 (1) ◽  
pp. 40-46
Author(s):  
V.O. DOROSCHUK ◽  
V.Ye. Sabko ◽  
O.V. Ivashko ◽  
L.O. POPOVA ◽  
A.S. Shalamay

A new method of enantioselective determination of S- and R-isomers of ibuprofen in human plasma by ultraperformance liquid chromatography with tandem mass spectrometric detection using solid-phase extraction was developed. For enantioselective separation of ibuprofen isomers, a LUX Cellulose-3 chiral chromatographic column was used. Complete separation of the enathiomer peaks is achieved in the isocratic elution conditions with a mobile phase ratio of 0.05 % formic acid solution (%): methanol (%) = 30 : 70 (v/v) and a flow rate of 0.2 mL/min. The mass spectrometric detection was performed at negative ionization mode with multiple reaction monitoring, using the transitions at 205.13 > 161.14 Da and 208.09 > 164.03 Da for ibuprofen enantiomers and deuterated ibuprofen (internal standard), respectively. The method validation included the evaluation of the selectivity, linearity, lower limit of quantification (LLOQ), within-run and between-run precision and accuracy. The LLOQ for the two enantiomers was 100 ng/mL in plasma. The calibration curves showed good linearity of each enantiomers in the ranges from 100 to 60000 ng/mL. The method was successfully applied to a pharmacokinetic study of ibuprofen enantiomers in human plasma.


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