scholarly journals Comparison of two sample preparation procedures for HPLC determination of ochratoxin A

2009 ◽  
Vol 61 (4) ◽  
pp. 639-644 ◽  
Author(s):  
Gorica Vukovic ◽  
Snezana Pavlovic ◽  
M.S. Ristic

In preparation of samples for chromatographic determination of ochratoxin A, two types of columns were used for sample cleanup (SPE and immunoaffinity columns). The first method consisted of liquid-liquid extraction with a mixture of chloroform and phosphoric acid, followed by ion-exchange cleanup on Waters Oasis MAX columns. The sec?ond method consisted of extraction with a mixture of water and methanol, followed by LCTech OtaCLEAN immunoaf?finity column cleanup. Recoveries of the methods were determined at three levels in three repetitions for maize flour, and they were 84% (%RSD = 19.2) for the first method of sample preparation and 101% (%RSD = 2.2) for the second method. Values of LOQ for OTA were 0.25 and 1.00 ?g/kg for the IAC and SPE clean-up procedures, respectively. Both methods comply with present regulations, but the MAX sample clean-up procedure should be used as an alternative, since the immunoaffinity column clean-up procedure is characterized by better reproducibility, accuracy, and efficiency.

Molecules ◽  
2019 ◽  
Vol 24 (15) ◽  
pp. 2761 ◽  
Author(s):  
Wenbin Chen ◽  
Siyuan Wu ◽  
Jianing Zhang ◽  
Fengjie Yu ◽  
Jianbo Hou ◽  
...  

In the present work, we developed a simple and rapid sample preparation method for the determination of neonicotinoid pesticides in honey based on the matrix-induced sugaring-out. Since there is a high concentration of sugars in the honey matrix, the honey samples were mixed directly with acetonitrile (ACN)-water mixture to trigger the phase separation. Analytes were extracted into the upper ACN phase without additional phase separation agents and injected into the HPLC system for the analysis. Parameters of this matrix-induced sugaring-out method were systematically investigated. The optimal protocol involves 2 g honey mixed with 4 mL ACN-water mixture (v/v, 60:40). In addition, this simple sample preparation method was compared with two other ACN-water-based homogenous liquid-liquid extraction methods, including salting-out assisted liquid-liquid extraction and subzero-temperature assisted liquid-liquid extraction. The present method was fully validated, the obtained limits of detection (LODs) and limits of quantification (LOQs) were from 21 to 27 and 70 to 90 μg/kg, respectively. Average recoveries at three spiked levels were in the range of 91.49% to 97.73%. Precision expressed as relative standard deviations (RSDs) in the inter-day and intra-day analysis were all lower than 5%. Finally, the developed method was applied for the analysis of eight honey samples, results showed that none of the target neonicotinoid residues were detected.


Química Nova ◽  
2012 ◽  
Vol 35 (2) ◽  
pp. 411-415 ◽  
Author(s):  
Sigrid Mennickent ◽  
Jonathan Contreras ◽  
Berta Schulz ◽  
Marta de Diego ◽  
Mario Vega

2017 ◽  
Vol 9 (36) ◽  
pp. 5395-5399 ◽  
Author(s):  
Ariane Isis Barros ◽  
Adriana Paiva de Oliveira ◽  
José Anchieta Gomes Neto ◽  
Ricardo Dalla Villa

Liquid–liquid extraction as a sample preparation procedure was employed for the determination of Na, K, Ca, and Mg in biodiesel by LS FAAS and Na and K by FP.


2019 ◽  
Vol 11 (37) ◽  
pp. 4835-4841 ◽  
Author(s):  
Wenbin Chen ◽  
Siyuan Wu ◽  
Jianing Zhang ◽  
Fengjie Yu ◽  
Xiaoqing Miao ◽  
...  

A simple, rapid, and effective sample preparation method was developed for the recovery of 5-hydroxymethylfurfural from honey samples with negligible co-extracted sugars.


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