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<p>Ochratoxin A (OTA) contamination in cocoa products may pose a food safety threat to consumers and compliance for international trade. To routinely monitor these commodities, an analytical method using liquid chromatography combined with immunoaffinity clean up and tandem mass spectrometry (LC-MS/MS) was developed in-house and successfully validated, offering a limit of quantification (LOQ) of 0.1&#xa0;µg/kg. Recovery experiments with OTA fortified samples (<i>n</i> = 27) in the range of 1–3&#xa0;µg/kg, resulted in an overall average recovery rate of 104% with extended uncertainty (U<sub>k=2</sub>) of 20%. Next, this method was applied to real cocoa powders (<i>n</i> = 26) and cocoa preparations (<i>n</i> = 15) bought from distinct supermarkets in Belgium. Most (90.2%) of examined samples were OTA contaminated (&gt; LOQ) with an average level of 1.1 ± 1.3&#xa0;µg/kg. Mean OTA level was significantly higher (<i>p</i> = 0.013) in cocoa powder samples (1.4 ± 1.6&#xa0;µg/kg, 92%) than in cocoa preparation samples (0.5 ± 0.3&#xa0;µg/kg, 87%). With the exception of 9.8% of the examined samples, OTA concentrations did not exceed the maximum permitted threshold of 3&#xa0;µg/kg set by European Regulation EU 2023/915. The highest level in contaminated samples was 6.5&#xa0;µg/kg, in cocoa powder, main ingredient used for cocoa preparation. Using these data, the probabilistic Monte Carlo simulation method was applied to estimate potential daily intakes for average and high cocoa consumption levels among adults (19–65 years) and the subsequent margin of exposure MoE (neoplastic and non-neoplastic) values were calculated. Based on the non-neoplastic endpoint (BMDL<sub>10</sub> = 4.73&#xa0;µg/kg BW) and neoplastic endpoint (BMDL<sub>10</sub> = 14.5&#xa0;µg/kg BW), the average and median MoE values were &gt; 200 and &gt; 10,000, respectively, for adult consumers, indicating a low health concern. Nevertheless, the high frequency of OTA-positive samples sold in Belgium is an important signal of attention for consumers that suggests an optimized frequency of surveillance according to European Regulations EU 2023/915 in order to reject the irregular batches of imported cocoa products.</p>

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Analysis of Ochratoxin A in commercial cocoa products: Intra-laboratory validation and estimation of potential dietary risk exposure in Belgium

  • 期刊论文

  • 发表日期：

    2025年12月12日

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  • EK Tangni,
  • J Laporte,
  • J Masquelier

摘要

Ochratoxin A (OTA) contamination in cocoa products may pose a food safety threat to consumers and compliance for international trade. To routinely monitor these commodities, an analytical method using liquid chromatography combined with immunoaffinity clean up and tandem mass spectrometry (LC-MS/MS) was developed in-house and successfully validated, offering a limit of quantification (LOQ) of 0.1 µg/kg. Recovery experiments with OTA fortified samples (n = 27) in the range of 1–3 µg/kg, resulted in an overall average recovery rate of 104% with extended uncertainty (Uk=2) of 20%. Next, this method was applied to real cocoa powders (n = 26) and cocoa preparations (n = 15) bought from distinct supermarkets in Belgium. Most (90.2%) of examined samples were OTA contaminated (> LOQ) with an average level of 1.1 ± 1.3 µg/kg. Mean OTA level was significantly higher (p = 0.013) in cocoa powder samples (1.4 ± 1.6 µg/kg, 92%) than in cocoa preparation samples (0.5 ± 0.3 µg/kg, 87%). With the exception of 9.8% of the examined samples, OTA concentrations did not exceed the maximum permitted threshold of 3 µg/kg set by European Regulation EU 2023/915. The highest level in contaminated samples was 6.5 µg/kg, in cocoa powder, main ingredient used for cocoa preparation. Using these data, the probabilistic Monte Carlo simulation method was applied to estimate potential daily intakes for average and high cocoa consumption levels among adults (19–65 years) and the subsequent margin of exposure MoE (neoplastic and non-neoplastic) values were calculated. Based on the non-neoplastic endpoint (BMDL10 = 4.73 µg/kg BW) and neoplastic endpoint (BMDL10 = 14.5 µg/kg BW), the average and median MoE values were > 200 and > 10,000, respectively, for adult consumers, indicating a low health concern. Nevertheless, the high frequency of OTA-positive samples sold in Belgium is an important signal of attention for consumers that suggests an optimized frequency of surveillance according to European Regulations EU 2023/915 in order to reject the irregular batches of imported cocoa products.