Pigmented oranges are a high value typical product, used for the production of healthy juice-based drinks due to the peculiar presence of anthocyanins as dietary antioxidants. A qualitative HPLC/PDA/MS analytical method for verifying presence/absence of blood orange anthocyanins was validated in accordance with Eurachem guide in terms of accordance (100%), specificity/selectivity, repeatability of retention time (CV < 0.5%), limit of detection (0.36 mg/L) and limit of decision (0.41 mg/L). Fifty commercial red orange juice beverages were collected on the market and analyzed to assess the occurrence of blood orange anthocyanins. The results showed that only 60% of analyzed products have a minimum content of anthocyanins of blood orange, guaranteeing the specifications of the product they publicize and sell until the expiration date. Therefore, it is possible to envisage a gradual degradation of the specific parameter (anthocyanins) or willful misconduct of producers (non-use of blood orange juice). In both cases, the consumer buys a product with high added value without such value being guaranteed. This information will be useful to revise the expiration date of these products, the percentage of blood orange juice used in the preparation and/or the storage conditions of the products.
OPEN ACCESSBeverages 2015, 1 83
An analytical method was developed for investigating aminocarminic acid occurrence in E120-labelled red-coloured-beverages and in E120 additives, with the aim of controlling the purity of the carmine additive in countries where the use of aminocarminic acid is forbidden. The carminic acid and the aminocarminic acid were separated by high-performance liquid chromatography-photodiode array-tandem mass spectrography (HPLC-PDA-MS/MS). The method was statistically validated. The regression lines, ranging from 10 to 100 mg/L, showed r(2 )> 0.9996. Recoveries from 97% to 101% were obtained for the fortification level of 50 mg/L; the relative standard deviations did not exceed 3%. The LODs were below 2 mg/L, whereas the LOQs did not exceed 4 mg/L. The method was successfully applied to 27 samples of commercial E120-labelled red-coloured beverages and E120 additives, collected in Italy during quality control investigations conducted by the Ministry. The results demonstrated that more than 50% of the samples contained aminocarminic acid, evidencing the alarming illicit use of this semi-synthetic carmine acid derivative.
A reversed phase high-performance liquid chromatographic method (HPLC/MS-MS) has been developed and validated for detection of alkaloids matrine and oxymatrine in fertilizer with labeled enhancer plant defense activities. The analytical method was validated statistically. The results show a strong matrix effect, requiring quantification by standard addition method. The regression lines showed r(2) > 0.994. Recoveries ranging from 97 to 104% were obtained for the fortification level of 0.01% wt wt(-1) and the relative standard deviations ranged from 3 to 4% (n = 10). The limits of detection were below 0.0001% wt wt(-1), while the limits of quantification did not exceed 0.0004% wt wt(-1). The method is currently applied in ICQRF Laboratory of Catania on fertilized and corroborant plant extract collected in the Italian market in the frame of MIPAAF institutional quality control activity, with the aim to dectect these unpermitted active substances.
This paper reports the occurrence of dehydroacetic acid in cheese and cheese coatings collected in Italy during Agricultural Ministry Official control. Dehydroacetic acid is an antimicrobial substance not allowed to be used in EU countries as a food additive, with unknown effects on human health. Dehydroacetic acid was measured by a validated HPLC method according to Commission Decision 2002/657/EC criteria in terms of specificity, linearity, precision and accuracy, limit of detection, and limit of quantification. The method was successfully applied to 129 samples of commercial cheese coatings and related treated cheeses collected in Italy during 2017. The overall results demonstrated that about 40% of the investigated cheese coatings contained dehydroacetic acid, ranging from 0.010% to 2.5% w/w, evidencing illicit employment of this substance. Moreover, about 25% of treated cheeses contained dehydroacetic acid, from 5 to 250 mg/Kg, proving transfer of this substance from crust to cheese.
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