Aflatoxins in Brazilian Peanut Confection

2016 ◽  
Vol 99 (3) ◽  
pp. 830-834 ◽  
Author(s):  
Maria H Iha ◽  
Isaura A Okada ◽  
Rita C Briganti ◽  
Camila A Mini ◽  
Mary W Trucksess
Keyword(s):  
Fluorescence Enhancement ◽  
Public Health Problem ◽  
Current Method ◽  
Immunoaffinity Column ◽  
Paulo State ◽  
Fluorescence Determination ◽  
The Mean ◽  
Aflatoxin B2 ◽  
Postcolumn Derivatization

Abstract The study's objectives were to evaluate a method for the determination of aflatoxins (AFs) in the Brazilian peanut confection “Paçoca” and to apply the method in investigating AF concentrations in Paçoca marketed in São Paulo State throughout 2013. Results of another survey conducted between 1994 and 2002 with another method were also reported. The current method consists of immunoaffinity column cleanup, LC with postcolumn derivatization for AF fluorescence enhancement, and fluorescence determination for the toxins. The mean recovery and mean RSDr values were 88.6 and 7.9%, respectively. The LODs for aflatoxin B1, aflatoxin B2, aflatoxin G1, and aflatoxin G2 were 0.04, 0.01, 0.02, and 0.01 ng/g; and the LOQs were 0.15, 0.04, 0.07, and 0.04 ng/g, respectively. Results of the two survey studies indicate that the contamination of AFs in Paçoca remains a public health problem. In the 2013 survey, 71 of 100 samples (71%) had AFs contamination ranging from 0.3 to 41.8 ng/g, with 12 samples (12%) containing >20 ng/g of the toxins, whereas in the 1994–2002 survey, 73 of 150 samples (51%) had AFs contamination ranging from 9 to 1439 ng/g with 65 samples (45%) containing levels >20 ng/g.

scholarly journals Determination of Aflatoxin in Processed Dried Cassava Root: Validation of a New Analytical Method for Cassava Flour

2010 ◽  
Vol 93 (6) ◽  
pp. 1882-1887 ◽  
Author(s):  
G J Benoit Gnonlonfin ◽  
David R Katerere ◽  
Yann Adjovi ◽  
Leon Brimer ◽  
Gordon S Shephard ◽  
...  
Keyword(s):  
Analytical Method ◽  
Optimal Performance ◽  
Immunoaffinity Column ◽  
Critical Factors ◽  
Toxin Concentration ◽  
Cassava Flour ◽  
Cassava Root ◽  
Fluorescence Determination ◽  
Postcolumn Derivatization

Abstract A new method that uses HPLC with a photochemical reactor for enhanced detection was developed and validated for the determination of aflatoxins in cassava flour. Samples were spiked with a mixture of four aflatoxins at 5, 10, and 20 g/kg mixed with either 1 or 5 g NaCl and extracted with methanolwater (80 20, v/v) by shaking for 10 or 30 min. An immunoaffinity column was used for cleanup. HPLC with postcolumn derivatization, for enhancement of aflatoxin fluorescence, and fluorescence determination were used for quantitation of the toxin concentration. The method was validated for recovery, linearity, and precision at the three concentrations tested. Recovery ranges were 5270, 6985, and 8089 for the spiking levels of 5.0, 10.0, and 20.0 g/kg, respectively. It appears that the amount of salt (NaCl) and the shaking time are critical factors in this method; optimal performance was obtained when 1 g salt was used and the shaking time was 10 min. The good linearity and precision of the method allowed baseline separation from interferences, e.g., coumarins.

Comparison of Postcolumn Derivatization-Liquid Chromatography with Thin-Layer Chromatography for Determination of Aflatoxins in Naturally Contaminated Corn

1990 ◽  
Vol 73 (4) ◽  
pp. 579-581 ◽  
Author(s):  
Rodney W Beaver ◽  
David M Wilson ◽  
Mary W Trucksess
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Correlation Coefficient ◽  
Low Levels ◽  
Aflatoxin B2 ◽  
Layer Chromatography ◽  
Postcolumn Derivatization

Abstract Quantitation of aflatoxins by liquid chromatography with postcolumn iodine derlvatization (LC-PCD) and fluorescence detection was compared with quantitation by the AOAC CB method, 968.22. Thirty-seven naturally contaminated corn samples were ground and then divided. One portion was extracted, and the extract was cleaned up and analyzed by thin-layer chromatography according to the CB method. The second portion was extracted and cleaned up In a similar fashion, but quantitation was by the LC-PCD method. For aflatoxin B1, concentrations ranging from 0 to 150 ng/g, results obtained by the 2 methods were fitted to a linear equation with the LC-PCD results as the dependent variable. The correlation coefficient was 0.99, the Intercept was near 0, and the slope was near 1. For aflatoxin B2, the correlation coefficient was 0.97, and the Intercept was near 0. However, the slope of the equation relating LC-PCD concentration to TLC concentration was only 0.5. We believe that this lack of equivalence between the methods for determination of aflatoxin B2 is due to overestlmatlon by the TLC method because the low levels present are near the TLC detection limit for B2.

scholarly journals Occurrence of aflatoxins in peanuts and peanut products determined by liquid chromatography with fluorescence detection

2013 ◽  
pp. 27-35 ◽  
Author(s):  
Biljana Stojanovska-Dimzoska ◽  
Zehra Hajrulai-Musliu ◽  
Elizabeta Dimitrieska-Stojkovic ◽  
Risto Uzunov ◽  
Pavle Sekulovski
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Limit Of Detection ◽  
Total Content ◽  
Immunoaffinity Column ◽  
Limit Of Quantification ◽  
Three Samples ◽  
The Mean ◽  
Positive Results

Liquid chromatography with fluorescence detection using immunoaffinity column clean-up was a method described for determination of aflatoxins (AFB1, AFB2, AFG1 and AFG2) in peanuts and peanut based products. The validation of the procedure was performed. Good coefficient of correlation was found for all aflatoxins in the range of 0.9993-0.9999. Limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.003-0.005 mg/kg and 0.009-0.023 mg/kg, respectively, which was acceptable. The mean recovery for total aflatoxins was 88.21%. The method also showed acceptable precision values in the range of 0.171-2.626% at proposed concentration levels for all four aflatoxins. RSDR values (within laboratory reproducibility) calculated from the results showed good correlation between two analysts for all aflatoxins and they ranged from 4.93-11.87%. The developed method was applied for the determination of aflatoxins in 27 samples of peanuts and peanut based products. The results showed that 21 peanut samples (77.7%) were below LOD of the method. Three samples had positive results over the MRL. There was one extreme value recorded for the total aflatoxins in peanut (289.2 mg/kg) and two peanut based products, peanut snack and peanut, with total content of aflatoxins being 16.3 mg/kg and 8.0 mg/kg, respectively. The obtained results demonstrated that the procedure was suitable for the de?termination of aflatoxins in peanuts and peanut based products and it could be implemented for the routine analysis.

scholarly journals Immunoaffinity Column Cleanup with Liquid Chromatography for Determination of Aflatoxin B1 in Corn Samples: Interlaboratory Study

2007 ◽  
Vol 90 (3) ◽  
pp. 765-772 ◽  
Author(s):  
Carlo Brera ◽  
Francesca Debegnach ◽  
Valentina Minardi ◽  
Elena Pannunzi ◽  
Barbara De Santis ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Aflatoxin B1 ◽  
Interlaboratory Study ◽  
Precolumn Derivatization ◽  
Immunoaffinity Column ◽  
Relative Standard ◽  
Postcolumn Derivatization

Abstract An interlaboratory study was conducted to evaluate the effectiveness of an immunoaffinity column cleanup liquid chromatography (LC) method for the determination of aflatoxin B1 levels in corn samples, enforced by European Union legislation. A test portion was extracted with methanolwater (80 + 20); the extract was filtered, diluted with phosphate-buffered saline solution, filtered on a microfiber glass filter, and applied to an immunoaffinity column. The column was washed with deionized water to remove interfering compounds, and the purified aflatoxin B1 was eluted with methanol. Aflatoxin B1 was separated and determined by reversed-phase LC with fluorescence detection after either pre- or postcolumn derivatization. Precolumn derivatization was achieved by generating the trifluoroacetic acid derivative, used by 8 laboratories. The postcolumn derivatization was achieved either with pyridinium hydrobromide perbromide, used by 16 laboratories, or with an electrochemical cell by the addition of bromide to the mobile phase, used by 5 laboratories. The derivatization techniques used were not significantly different when compared by the Student's t-test; the method was statistically evaluated for all the laboratories. Five corn sample materials, both spiked and naturally contaminated, were sent to 29 laboratories (22 Italian and 7 European). Test portions were spiked with aflatoxin B1 at levels of 2.00 and 5.00 ng/g. The mean values for recovery were 82% for the low level and 84% for the high contamination level. Based on results for spiked samples (blind pairs at 2 levels) as well as naturally contaminated samples (blind pairs at 3 levels), the values for relative standard deviation for repeatability (RSDr) ranged from 9.9 to 28.7%. The values for relative standard deviation for reproducibility (RSDR) ranged from 18.6 to 36.8%. The method demonstrated acceptable within- and between-laboratory precision for this matrix, as evidenced by the HorRat values.

scholarly journals Determination of Aflatoxins and Ochratoxin a in Animal Liver Using HPLC-FD Method with Immunoaffinity Column Clean-Up

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Biljana Stojanovska-Dimzoska ◽  
Elizabeta Dimitrieska-Stojkovic ◽  
Zehra Hajrulai-Musliu ◽  
Risto Uzunov ◽  
Aleksandra Angeleska ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Ochratoxin A ◽  
Immunoaffinity Column ◽  
Acceptable Range ◽  
Animal Liver ◽  
Relative Standard ◽  
Validation Parameters ◽  
The Mean ◽  
Concentration Levels

Abstract Analytical methods based on immunoaffinity column clean-up and quantitative determination with liquid chromatography-fluorescence detection were used to determine aflatoxins and ochratoxin A in liver samples. The validation of the procedures was performed. The linearity of the methods was checked, and a good coefficient of correlation was found for all aflatoxins and OTA as well. The LOD and LOQ were acceptable: 0.003 µg/kg and 0.009 µg/kg for AFB1; 0.001 µg/kg and 0.005 µg/kg for AFB2; 0.006 µg/kg and 0.020 µg/kg for AFG1; 0.007 µg/kg and 0.022 µg/kg for AFG2; 0.08 µg/kg and 0.27 µg/kg for OTA. The results for the repeatability estimated by the relative standard deviation (RSDr) were satisfactory and the obtained values were in the acceptable range (1.97–14.41% for all aflatoxins and 3.76-8.31% for OTA) at three proposed concentration levels. RSDR values showed acceptable correlation between two analysts for all four aflatoxins and OTA. The RSDR values were as followed: 2.37% and 5.60% for AFB1, 6.71% and 8.78% for AFB2, 4.40% and 7.00% for AFG1 and 10.30% and 13.91% for AFG2 (for the first and second analyst, respectively). The RSDR values for OTA were 4.91% and 3.15% (1 µg/kg); 3.76% and 4.12% (5 µg/kg) and 8.31% and 8.21% (10 µg/kg). The mean recovery for total aflatoxins and OTA were 78.10% and 93.34%, respectively. All validation parameters were in accordance to European legislation. They indicate that the proposed analytical procedures are suitable and they could be methods of choice for the determination of aflatoxins and OTA in liver samples.

Determination of Chloramphenicol Residues in Aquatic Products Using Immunoaffinity Column Cleanup and High Performance Liquid Chromatography with Ultraviolet Detection

2013 ◽  
Vol 96 (4) ◽  
pp. 897-901 ◽  
Author(s):  
Qing-Jie Zhang ◽  
Tao Peng ◽  
Dong-Dong Chen ◽  
Jie Xie ◽  
Xiong Wang ◽  
...  
Keyword(s):  
High Performance ◽  
Low Cost ◽  
Ammonium Hydroxide ◽  
Optimal Conditions ◽  
Immunoaffinity Column ◽  
Ultraviolet Detection ◽  
Aquatic Products ◽  
Highly Sensitive ◽  
The Mean

Abstract A method based on HPLC with UV detection was developed for the quantitative determination of chloramphenicol (CAP) residues in aquatic products. The samples were extracted with ethyl acetate–ammonium hydroxide (98 + 2, v/v), followed by a cleanup step using an immunoaffinity column. The analytes were determined by HPLC-UV. Optimal conditions for the extraction and cleanup procedures are described. The linear regression equation was y = 91.47x – 8.60 with R2 = 0.9998 (y = peak area and x = CAP concentration) and showed a good reproducibility. The LOQ was 0.25 μg/kg for determining CAP spiked in the aquatic products. The mean recoveries of CAP from fish and shrimp samples fortified at 0.25–1.0 μg/kg were 88.7–93.1 and 92.0–97.3%, respectively; the repeatability RSDs were less than 8.1%. It was concluded that the method is simple, highly sensitive, and low cost for quantitatively measuring CAP residues in aquatic products. Analyte identification was confirmed by HPLC/MS/MS analysis.

Determination of Semduramicin Sodium in Poultry Liver by Liquid Chromatography with Vanillin Postcolumn Derivatization

1994 ◽  
Vol 77 (3) ◽  
pp. 577-582 ◽  
Author(s):  
Jon F Ericson ◽  
Albert Calcagni ◽  
Martin J Lynch
Keyword(s):  
Liquid Chromatography ◽  
Quantitative Determination ◽  
Solid Phase ◽  
Ammonium Hydroxide ◽  
Phase Extraction ◽  
Minimum Level ◽  
The Mean ◽  
Liquid Chromatographic ◽  
Postcolumn Derivatization

Abstract A liquid chromatographic (LC) method is described for the quantitative determination of semduramicin sodium in broiler liver when administered under projected use conditions. For this procedure, semduramicin sodium is extracted from liver with methanolic ammonium hydroxide, separated and concentrated by solid-phase extraction steps, and determined by LC with postcolumn derivatization with vanillin. The mean recovery of drug was 95% over the 40-320 ng/g range, the coefficient of variation was ±10% or better, and no interference was observed from commercial poly ether ionophores. The minimum level of detection for semduramicin sodium in broiler liver is 25 ng/g.

Determination of Aflatoxins B1, B2, G1, and G2 in Olive Oil, Peanut Oil, and Sesame Oil Using Immunoaffinity Column Cleanup, Postcolumn Derivatization, and Liquid Chromatography/Fluorescence Detection: Collaborative Study

2012 ◽  
Vol 95 (6) ◽  
pp. 1689-1700 ◽  
Author(s):  
Lei Bao ◽  
Chengzhu Liang ◽  
Mary W Trucksess ◽  
Yanli Xu ◽  
Ning Lv ◽  
...  
Keyword(s):  
Olive Oil ◽  
Lower Layer ◽  
Collaborative Study ◽  
Sesame Oil ◽  
Peanut Oil ◽  
Immunoaffinity Column ◽  
Fluorescence Detector ◽  
Repeatability And Reproducibility ◽  
Postcolumn Derivatization

Abstract The accuracy, repeatability, and reproducibility characteristics of a method using immunoaffinity column (IAC) cleanup with postcolumn derivatization and LC with a fluorescence detector (FLD) for determination of aflatoxins (AFs; sum of AFs B1, B2, G1, and G2) in olive oil, peanut oil, and sesame oil have been established in a collaborative study involving 15 laboratories from six countries. Blind duplicate samples of blank, spiked at levels ranging from 0.25 to 20.0 μg/kg for AF, were analyzed. A naturally contaminated peanut oil sample was also included. Test samples were extracted with methanol–water (55 + 45, v/v). After shaking and centrifuging, the lower layer was filtered, diluted with water, and filtered through glass microfiber filter paper. The filtrate was then passed through an IAC, and the toxins were eluted with methanol. The toxins were then subjected to RPLC-FLD analysis after postcolumn derivatization. Average recoveries of AFs from olive oil, peanut oil, and sesame oil ranged from 84 to 92% (at spiking levels ranging from 2.0 to 20.0 μg/kg); of AFB1 from 86 to 93% (at spiking levels ranging from 1.0 to 10.0 μg/kg); of AFB2 from 89 to 95% (at spiking levels ranging from 0.25 to 2.5 μg/kg); of AFG1 from 85 to 97% (at spiking levels ranging from 0.5 to 5.0 μg/kg); and of AFG2 from 76 to 85% (at spiking levels ranging from 0.25 to 2.5 μg/kg). RSDs for within-laboratory repeatability (RSDr) ranged from 3.4 to 10.2% for AF, from 3.5 to 10.9% for AFB1, from 3.2 to 9.5% for AFB2, from 6.5 to 14.9% for AFG1, and from 4.8 to 14.2% for AFG2. RSDs for between-laboratory reproducibility (RSDR) ranged from 6.1 to 14.5% for AF, from 7.5 to 15.4% for AFB1, from 7.1 to 14.6% for AFB2, from 10.8 to 18.1% for AFG1, and from 7.6 to 23.7% for AFG2. Horwitz ratio values were ≤2 for the analytes in the three matrixes.

Sign in / Sign up

Export Citation Format

Share Document