scholarly journals NanoMIP-Based Solid Phase Extraction of Fluoroquinolones from Human Urine: A Proof-of-Concept Study

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.

2012 ◽  
Vol 62 (2) ◽  
pp. 211-220 ◽  
Author(s):  
Jasmina Tonic-Ribarska ◽  
Arlinda Haxhiu ◽  
Zoran Sterjev ◽  
Gordana Kiteva ◽  
Ljubica Suturkova ◽  
...  

Development and validation of a bioanalytical LC-UV method with solid-phase extraction for determination of valproic acid in saliva A bioanalytical HPLC method with UV detection for the determination of the antiepileptic drug valproic acid in human saliva has been developed and validated. Saliva represents an alternative matrix for therapeutic monitoring of antiepileptic drugs due to the increasing interest in free drug concentration. The proposed method involved solid-phase extraction for sample preparation and yielded very good mean recoveries of 99.4 % and 97.9 % for valproic acid and IS, respectively. The calibration function for valproic acid was linear over the concentration range of 1.0-50.0 μg mL-1 (R2 = 0.9989). Within-run and between-run precision and accuracy were studied at four concentrations and RSDs were less than 7.3 and 2.2 %, while accuracy values were higher than 96.8 and 97.5 %, respectively. The described method provides sensitivity, linearity, precision, accuracy and is suitable for analyses of valproic acid in saliva samples.


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