Application of experimental design in optimization of solid phase extraction of mycophenolic acid and mycophenolic acid glucuronide from human urine and plasma and SPE-RP-HPLC method validation

2008 ◽  
Vol 47 (3) ◽  
pp. 575-585 ◽  
Author(s):  
Ljiljana Živanović ◽  
Ana Ličanski ◽  
Mira Zečević ◽  
Biljana Jocić ◽  
Mirjana Kostić
Separations ◽  
2021 ◽  
Vol 8 (11) ◽  
pp. 226
Author(s):  
Matteo Chiarello ◽  
Laura Anfossi ◽  
Simone Cavalera ◽  
Fabio Di Di Nardo ◽  
Thea Serra ◽  
...  

NanoMIPs that are prepared by solid phase synthesis have proven to be very versatile, but to date only limited attention has been paid to their use in solid phase extraction. Thus, since nanoMIPs show close similarities, in terms of binding behavior, to antibodies, it seems relevant to verify if it is possible to use them as mimics of the natural antibodies that are used in immunoextraction methods. As a proof-of-concept, we considered prepared nanoMIPs against fluoroquinolone ciprofloxacin. Several nanoMIPs were prepared in water with polymerization mixtures of different compositions. The polymer with the highest affinity towards ciprofloxacin was then grafted onto a solid support and used to set up a solid phase extraction–HPLC method with fluorescence detection, for the determination of fluoroquinolones in human urine. The method resulted in successful selection for the fluoroquinolone antibiotics, such that the nanoMIPs were suitable for direct extraction of the antibiotics from the urine samples at the µg mL−1 level. They required no preliminary treatment, except for a 1 + 9 (v/v) dilution with a buffer of pH 4.5 and they had good analyte recovery rates; up to 85% with precision in the range of 3 to 4.5%, without interference from the matrix. These experimental results demonstrate, for the first time, the feasibility of the use of nanoMIPs to develop solid phase extraction methods.


2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Paras P. Vekariya ◽  
Hitendra S. Joshi

Simple and rapid reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated using solid phase extraction (SPE) technique for the determination of Azilsartan Medoxomil Potassium (AMP) in human plasma; detection was carried out by photo diode array detector. Chromatographic separation of the analyte AMP was achieved within 7.5 min by Waters symmetry C18 (4.6 × 250 mm, 5 µm) column, mobile phase was 25 mM ammonium acetate buffer (pH 5.5): acetonitrile 55 : 45 v/v, flow rate was 1.0 mL/min, and the detection was carried out at 254 nm. Calibration curve was linear (r2 > 0.9985) in the range of 1.0–9.0 µg/mL, limit of detection (LOD) and limit of quantitation (LOQ) were 0.150 µg/mL and 0.400 µg/mL, respectively, and intra- and interday deviations were between 1.53–8.41% and 1.78–4.59%, respectively. The overall mean recovery of AMP was 92.35%. No any endogenous constituents were found to interfere at retention time of the analyte. This new RP-HPLC method was successfully validated and may be applied to conduct bioavailability and bioequivalence studies of AMP.


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