Dehydroacetic acid in cheese and cheese coating, results of official control in Italy.

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.

Matrine and oxymatrine in corroborant plant extracts and fertilizers: HPLC/MS-MS method development and single-laboratory validation.

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.

Survey of neonicotinoids and fipronil in corn seeds for agriculture.

Recently, legislative decisions withdrew or temporarily suspended the use of neonicotinoids and fipronil as seeds tanning in many countries because of their endocrine-disrupting activity imputable to the bees' toxicity. In this study, the occurrence of acetamiprid, fipronil, clothianidin, flonicamid, imidacloprid, nitenpyram, thiacloprid and thiamethoxam was detected in 66 samples of commercial treated corn seeds, collected in the Italian market in the frame of ministerial institutional quality control activity. Because of the lack of a validated analytical protocol for neonicotinoid detection in seeds, a routinely suitable liquid chromatography-tandem mass spectroscopy (LC-MS/MS) analytical method was developed and statistically validated on fortified corn seeds.

UHPLC/MS-MS Analysis of Six Neonicotinoids in Honey by Modified QuEChERS: Method Development, Validation, and Uncertainty Measurement.

Rapid and reliable multiresidue analytical methods were developed and validated for the determination of 6 neonicotinoids pesticides (acetamiprid, clothianidin, imidacloprid, nitenpyram, thiacloprid, and thiamethoxam) in honey. A modified QuEChERS method has allowed a very rapid and efficient single-step extraction, while the detection was performed by UHPLC/MS-MS. The recovery studies were carried out by spiking the samples at two concentration levels (10 and 40 μg/kg).

Aminocarminic acid in E120-labelled food additives and beverages.

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.

Determination of volatile compounds in wine by gas chromatography-flame ionization detection: comparison between the U.S. Environmental Protection Agency 3sigma approach and Hubaux-Vos calculation of detection limits using ordinary and bivariate least squares.

A capillary GC-flame ionization detection (FID) method to determine volatile compounds (ethyl acetate, 1,1-diethoxyethane, methyl alcohol, 1-propanol, 2-methyl-1-propanol, 2-methyl-1-butanol, 3-methyl-1-butanol, 1-butanol, and 2-butanol) in wine was investigated in terms of calculation of detection limits and calibration method. The main objectives were: (1) calculation of regression coefficient parameters by ordinary least-squares (OLS) and bivariate least-squares (BLS) regression models, taking into account errors in both axes; (2) estimation of linear dynamic range (LDR) according to International Conference on Harmonization recommendations; (3) performance evaluation of a method by using three different internal standards (ISs) such as acetonitrile, acetone, and 1-pentanol; (4) evaluation of LODs according to the U.S.

Gas chromatographic quantitative analysis of methanol in wine: operative conditions, optimization and calibration model choice.

The influence of the wine distillation process on methanol content has been determined by quantitative analysis using gas chromatographic flame ionization (GC-FID) detection. A comparative study between direct injection of diluted wine and injection of distilled wine was performed. The distillation process does not affect methanol quantification in wines in proportions higher than 10%.

HPLC/PDA/ESI-MS evaluation of saffron (Crocus sativus L.) adulteration.

The present study evaluated the reliability of the ISO/TS 3632-2 UV-Vis spectrometric method for saffron classification, making experiments on saffron samples to which were added increasing concentrations of common saffron spice adulterants (safflower, marigold and turmeric). The results showed that the ISO/TS 3632-2 method is not able to detect addition of up to 10-20%, w/w, of saffron adulterants. For additions from 20 to 50%, w/w, of the three adulterants, saffron was classified in a wrong category; addition of higher than 50%, w/w, determined variations in the investigated parameters that did not allow identification of the product as "saffron".

Characterization of polyphenolic compounds in unripe chinotto (Citrus myrtifolia) fruit by HPLC/PDA/ESI/MS-MS.

The flavonoid and furocoumarin composition was investigated of peel and pulp tissues of unripe fruits of Citrus myrtifolia Rafinesque, an ingredient of the popular soft drink "chinotto". Compound separation and identification was made using an HPLC-PDA detector coupled to ESI/MS/MS in positive and negative mode. Eighteen compounds (3-hydroxy-3-methylglutaryl-, C- and O-glycosyl flavonoids, furocoumarins and polymethoxylated flavones) were identified and quantified.

Determination of plant hormones in fertilizers by high-performance liquid chromatography with photodiode array detection: method development and single-laboratory validation.

A simple and reliable high-performance liquid chromatographic method that uses photodiode array detection was developed for the simultaneous determination of 12 native and synthetic plant hormones, i.e., plant growth regulators (PGRs), in fertilizers, such as 1-naphthol, 2,4-dichlorophenoxyacetic acid, 4-(2,4-dichlorophenoxy)butyric acid, 4-chlorophenoxyacetic acid, indole-3-acetic acid, 4-(3-indolyl)butyric acid, dichlorprop, (4-chloro-2-methylphenoxy)acetic acid, alpha-naphthaleneacetic acid, 1-naphthaleneacetamide, beta-naphthoxyacetic acid, and thidiazuron.