Molecularly imprinted polymer for selective extraction of 3-methylflavone-8-carboxylic acid from human urine followed by its determination using zwitterionic hydrophilic interaction liquid chromatography

2011 ◽  
Vol 34 (22) ◽  
pp. 3265-3271 ◽  
Author(s):  
Ramisetti N. Rao ◽  
Pawan K. Maurya ◽  
Ramakrishna Kuntamukkala ◽  
Wani D. Vitthal ◽  
Murali V. N. K. Talluri
2021 ◽  
Vol 11 (4) ◽  
pp. 1577
Author(s):  
Marco Mora-Granados ◽  
David González-Gómez ◽  
Jin Su Jeong ◽  
Alejandrina Gallego-Picó

Studies for monitoring the bioavailability of dietary flavonoid compounds generate great interest. Among them, low-molecular-weight phenolic acids, secondary metabolites present in colonic catabolism and urinary excretion, have been proposed as biomarkers of polyphenol intake. Using 4-hydroxyphenylacetic acid as a template, a molecularly imprinted polymer (MIP) was synthesized for selective extraction of these hydroxylated metabolites from human urine samples and posterior analysis in an HPLC-DAD-MS system. Polymers were characterized by Scanning electron microscopy (SEM), Attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR), Brunauer-Emmett-Teller (BET) method, and binding experiments. MIP presents specific recognition ability for template and analogues molecules. This capacity of recognition and the pH dependence of the binding strength was also studied. The method was validated over a concentration range of 0.25–40 mg/L, r2 > 0.995. In the optimized conditions, the recovery value was 94% with RSD 1.2%. The Limit of Detection (LOD) and Limit of Quantification (LOQ) were 1.22 and 3.69 mg/L, respectively. In our knowledge, it is the first time that this methodology is applied to analyze urinary catabolites of the polyphenol compound and to provide a specific method and simple analysis alternative. The selective extraction of these metabolites improves the application and results obtained by other less sensitive analysis methods than the validation method. It also facilitates the development of new screening methods.


2015 ◽  
Vol 8 (1) ◽  
pp. 37-43 ◽  
Author(s):  
L. Xie ◽  
P. Sheng ◽  
W. Kong ◽  
X. Zhao ◽  
Z. Ou-Yang ◽  
...  

A rapid, selective and reliable sample preparation technique employing solid-phase extraction (SPE) based on molecularly imprinted polymer (MIP) for the determination of ochratoxin A (OTA) in human urine was described. After sample adjustment to pH 2.5 with 0.1 M HCl, the urine sample was loaded onto the MIP-SPE column, and after a wash step, OTA was eluted for measurement by ultra-high performance liquid chromatography coupled with fluorescence detection. Key parameters which affected the MIP-SPE extraction efficiency were optimized as was the detection method. Under the optimised conditions, the limits of detection and quantification for OTA in urine were 0.2 ng/ml and 0.6 ng/ml, respectively. The recoveries for OTA in urine, spiked at the 0.6, 6.0 and 60 ng/ml levels, ranged from 92.0 to 98.9%. Sixty urine samples were analysed, of which four were found to contain OTA at concentrations ranging from 0.022 to 0.083 ng/ml; the positive results were confirmed by liquid chromatography coupled with tandem mass spectrometry. OTA determination in urine is a good indicator for human exposure to the mycotoxin, and this is the first report on OTA contamination in Chinese people.


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