Mycotoxin risk assessment for consumers of groundnut in domestic markets in Nigeria.

The fungal and multi-mycotoxin profiles of groundnuts sold in domestic markets in Nigeria as well as the associated risk to consumers were assessed in the present study. Four hundred fungal isolates representing mainly Aspergillus [58.6%: Aspergillus section Flavi (37.1%) and A. niger-clade (21.5%)], Penicillium (40.9%) and Fusarium (0.5%) were isolated from 82 (97.6%, n=84) groundnut samples collected from four agro-ecological zones (AEZs) of Nigeria. The incidence of aflatoxin-producing A. flavus isolates (71%) was significantly (p<0.05) higher in the groundnuts than that of the non-aflatoxigenic isolates (29%). Fifty-four fungal metabolites [including aflatoxins (AFB1, AFB2, AFG1, AFG2 and AFM1), beauvericin (BEAU), cyclopiazonic acid (CPA), moniliformin, nivalenol and ochratoxin A] and four bacterial metabolites were detected in the groundnuts by liquid chromatography tandem mass spectrometry. Aflatoxins (39%; max: 2076µg/kg; mean: 216µg/kg) were detected in more samples than any other mycotoxin. About 25, 23 and 14% of the samples respectively were above the 2µg/kg AFB1, 4 and 20µg/kg total aflatoxin limits of the European Union and US FDA respectively. The mean margins of exposure of AFB1 and total aflatoxins for adult consumers were 1665 and 908, respectively, while mean estimated daily intake values for infants, children and adults were <0.1% for BEAU and 4% for CPA. Consumers of mycotoxin contaminated groundnuts in Nigeria may therefore be at a risk of liver cancer in addition to other combinatory effects of mycotoxin/metabolite cocktails. There is need for increased targeted interventions in the groundnut value chain in Nigeria for public health benefits.

Quantitative assessment of moniliformin in cereals via alternative precipitation pathways, aided by LC-LIT-MS and LC-Q-TOF-MS.

The availability of a simple chemical precipitation workflow aided by targeted and untargeted mass spectrometry would provide an accurate diagnostic platform for the direct determination of moniliformin in cereals for food safety control. In-house method validation was performed at six concentration levels of 8, 40, 80, 200, 400, and 600 ng g(-1) in cereal flours of wheat, corn, rye, oats and barley. Spiking experiments were made at three concentration levels of 20, 40 and 100 ng g(-1). Protein precipitation and "PHREE" column cleanup strategy provided recoveries of 81-108% for all cereals matrices using external calibrants. "PHREE" purification provided significant (p < 0.05) ion signal enhancement reduction advantage for all matrices except corn flour. Moniliformin underwent significant (p < 0.05) degradation over 2 weeks when prepared in acidified water. A simple, low-cost and fit-for-purpose procedure for the identification and quantitation of moniliformin in cereals becomes available to support prospective regulatory function.

Monitoring of 29 weight loss compounds in foods and dietary supplements by LC-MS/MS.

Because of the rapid growth in dietary supplement availability and public concern for weight control, the investigation of foods and various dietary supplements illegally adulterated with weight loss compounds has become increasingly important. A total of 29 weight loss compounds, including sennoside, sibutramine, ephedrine and their analogues, found to be adulterated in foods and dietary supplements were simultaneously examined by LC-MS/MS. The 188 samples were collected between 2009 and 2012 in South Korea, and method validation was performed to determine the adulterants to the weight loss compounds. LODs, LOQs and linearity ranged from 0.03 to 7.5 ng ml⁻¹, from 0.08 to 30.00 ng ml⁻¹, and from 0.990 to 0.999, respectively. The results showed that nine weight loss compounds, namely bisacodyl, desmethylsibutramine, didesmethylsibutramine, ephedrine, fluoxetine, pseudoephedrine, sennoside A, sennoside B and sibutramine, were detected in 62 of all collected samples and were found in order of frequency as follows: sibutramine, 25.7%; sennoside A, 22.9%; sennoside B, 20.0%; fluoxetine, 8.6%; desmethylsibutramine, 7.1%; bisacodyl, ephedrine, and pseudoephedrine, 4.3%; and didesmethylsibutramine, 2.9%. Sibutramine, which was the most frequently found adulterant, ranged in levels from 0.03 to 132.40 mg g⁻¹ (2010), from 0.88 to 76.2 mg g⁻¹ (2011), and from 0.07 to 0.24 mg g⁻¹ (2012). Although the concentrations of most compounds ranged widely, some compounds such as bisacodyl and fluoxetine were found at high concentrations in several samples.

Determination of PDE-5 inhibitors and appetite suppressants in adulterated dietary supplements using LC/PDA and LC/MS.

There have been a number of reports of dietary supplements contaminated with illegal adulterants that threaten consumers' health because of their adverse pharmacological effects. In the present study, a convenient and economic method was developed to detect illegal pharmaceutics, such as PDE-5 inhibitor and appetite suppressants, using liquid chromatography (LC)/photodiode array (PDA) for screening and LC/mass spectrometry (MS) for successive confirmation. Target peaks were identified by comparison of their chromatographic retention times and PDA spectra with those of synthetic standards and finally confirmed by LC/MS. As a result, tadalafil, a PDE-5 inhibitor, and N-desmethylsibutramine, a derivative of sibutramine, were detected in various dietary supplements at concentrations of 13.5-21.9 mg and 3.0 mg per single dose, respectively. The present study will contribute to the development of an analytical method enabling rapid screening of a variety of health foods, and the result suggests that consumers should be aware of serious health risks related to these illegal compounds.