Validation of a Simple and Reliable Method for the Determination of Aflatoxins in Soil and Food Matrices
Aflatoxins (AFs) are toxic fungal secondary metabolites that are commonly detected in food commodities. Currently, there is a lack of generic methods capable of determining AFs both at postharvest stages in agricultural products and preharvest stages, namely, the agricultural soil. Here, we present...
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| Published in | ACS omega Vol. 6; no. 29; pp. 18684 - 18693 |
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| Main Authors | , , , , , |
| Format | Journal Article |
| Language | English |
| Published |
American Chemical Society
27.07.2021
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| Abstract | Aflatoxins (AFs) are toxic fungal secondary metabolites that are commonly detected in food commodities. Currently, there is a lack of generic methods capable of determining AFs both at postharvest stages in agricultural products and preharvest stages, namely, the agricultural soil. Here, we present a simple and reliable method for quantitative analysis of AFs in soil and food matrices at environmentally relevant concentrations for the first time, using the same extraction procedure and chromatography, either by HPLC-FLD or LC–MS. AFs were extracted from matrices by ultrasonication using an acetonitrile/water mixture (84:16, v + v) without extensive and time-consuming cleanup procedures. Food extracts were defatted with n-hexane. Matrix effects in terms of signal suppression/enhancement (SSE) for HPLC-FLD were within ±20% for all matrices tested. For LC–MS, the SSE values were mostly within ±20% for soil matrices but outside ±20% for all food matrices. The sensitivity of the method allowed quantitative analysis even at trace levels with quantification limits (LOQs) between 0.04 and 0.23 μg kg–1 for HPLC-FLD and 0.06–0.23 μg kg–1 for LC–MS. The recoveries ranged from 64 to 92, 74 to 101, and 78 to 103% for fortification levels of 0.5, 5, and 20 μg kg–1, respectively, with repeatability values of 2–18%. The validation results are in accordance with the quality criteria and limits for mycotoxins set by the European Commission, thus confirming a satisfactory performance of the analytical method. Although reliable analysis is possible with both instruments, the HPLC-FLD method may be more suitable for routine analysis because it does not require consideration of the matrix. |
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| AbstractList | Aflatoxins (AFs)
are toxic fungal secondary metabolites that are
commonly detected in food commodities. Currently, there is a lack
of generic methods capable of determining AFs both at postharvest
stages in agricultural products and preharvest stages, namely, the
agricultural soil. Here, we present a simple and reliable method for
quantitative analysis of AFs in soil and food matrices at environmentally
relevant concentrations for the first time, using the same extraction
procedure and chromatography, either by HPLC-FLD or LC–MS.
AFs were extracted from matrices by ultrasonication using an acetonitrile/water
mixture (84:16, v + v) without extensive and time-consuming cleanup
procedures. Food extracts were defatted with
n
-hexane.
Matrix effects in terms of signal suppression/enhancement (SSE) for
HPLC-FLD were within ±20% for all matrices tested. For LC–MS,
the SSE values were mostly within ±20% for soil matrices but
outside ±20% for all food matrices. The sensitivity of the method
allowed quantitative analysis even at trace levels with quantification
limits (LOQs) between 0.04 and 0.23 μg kg
–1
for HPLC-FLD and 0.06–0.23 μg kg
–1
for LC–MS. The recoveries ranged from 64 to 92, 74 to 101,
and 78 to 103% for fortification levels of 0.5, 5, and 20 μg
kg
–1
, respectively, with repeatability values of
2–18%. The validation results are in accordance with the quality
criteria and limits for mycotoxins set by the European Commission,
thus confirming a satisfactory performance of the analytical method.
Although reliable analysis is possible with both instruments, the
HPLC-FLD method may be more suitable for routine analysis because
it does not require consideration of the matrix. Aflatoxins (AFs) are toxic fungal secondary metabolites that are commonly detected in food commodities. Currently, there is a lack of generic methods capable of determining AFs both at postharvest stages in agricultural products and preharvest stages, namely, the agricultural soil. Here, we present a simple and reliable method for quantitative analysis of AFs in soil and food matrices at environmentally relevant concentrations for the first time, using the same extraction procedure and chromatography, either by HPLC-FLD or LC–MS. AFs were extracted from matrices by ultrasonication using an acetonitrile/water mixture (84:16, v + v) without extensive and time-consuming cleanup procedures. Food extracts were defatted with n-hexane. Matrix effects in terms of signal suppression/enhancement (SSE) for HPLC-FLD were within ±20% for all matrices tested. For LC–MS, the SSE values were mostly within ±20% for soil matrices but outside ±20% for all food matrices. The sensitivity of the method allowed quantitative analysis even at trace levels with quantification limits (LOQs) between 0.04 and 0.23 μg kg–1 for HPLC-FLD and 0.06–0.23 μg kg–1 for LC–MS. The recoveries ranged from 64 to 92, 74 to 101, and 78 to 103% for fortification levels of 0.5, 5, and 20 μg kg–1, respectively, with repeatability values of 2–18%. The validation results are in accordance with the quality criteria and limits for mycotoxins set by the European Commission, thus confirming a satisfactory performance of the analytical method. Although reliable analysis is possible with both instruments, the HPLC-FLD method may be more suitable for routine analysis because it does not require consideration of the matrix. |
| Author | Schaumann, Gabriele E Dahlke, Niklaus R. P Albert, Julius Muñoz, Katherine More, Camilla A Steinmetz, Zacharias |
| AuthorAffiliation | iES Landau, Institute for Environmental Sciences, Group of Organic and Ecological Chemistry University of Koblenz-Landau iES Landau, Institute for Environmental Sciences, Group of Environmental and Soil Chemistry |
| AuthorAffiliation_xml | – name: iES Landau, Institute for Environmental Sciences, Group of Environmental and Soil Chemistry – name: iES Landau, Institute for Environmental Sciences, Group of Organic and Ecological Chemistry – name: University of Koblenz-Landau |
| Author_xml | – sequence: 1 givenname: Julius orcidid: 0000-0001-5468-6069 surname: Albert fullname: Albert, Julius organization: University of Koblenz-Landau – sequence: 2 givenname: Camilla A surname: More fullname: More, Camilla A organization: University of Koblenz-Landau – sequence: 3 givenname: Niklaus R. P surname: Dahlke fullname: Dahlke, Niklaus R. P organization: University of Koblenz-Landau – sequence: 4 givenname: Zacharias orcidid: 0000-0001-6675-5033 surname: Steinmetz fullname: Steinmetz, Zacharias organization: University of Koblenz-Landau – sequence: 5 givenname: Gabriele E orcidid: 0000-0003-1788-2751 surname: Schaumann fullname: Schaumann, Gabriele E email: Schaumann@uni-landau.de organization: University of Koblenz-Landau – sequence: 6 givenname: Katherine surname: Muñoz fullname: Muñoz, Katherine organization: University of Koblenz-Landau |
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| Snippet | Aflatoxins (AFs) are toxic fungal secondary metabolites that are commonly detected in food commodities. Currently, there is a lack of generic methods capable... Aflatoxins (AFs) are toxic fungal secondary metabolites that are commonly detected in food commodities. Currently, there is a lack of generic methods capable... |
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| Title | Validation of a Simple and Reliable Method for the Determination of Aflatoxins in Soil and Food Matrices |
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