It indicated that the free amino acid profile determined by HPLC-FLD can provide sufficient information to discriminate honey samples according to their botanical origins. © 2016 Society of Chemical Industry.

A potential method for the discrimination and prediction of honey samples of various botanical origins was developed based on the non-targeted volatile profiles obtained by solid-phase microextraction with gas chromatography and mass spectrometry combined with chemometrics. The blind analysis of non-targeted volatile profiles was carried out using solid-phase microextraction with gas chromatography and mass spectrometry for 87 authentic honey samples from four botanical origins (acacia, linden, vitex, and rape). The number of variables was reduced from 2734 to 70 by using a series of filters. Based on the optimized 70 variables, 79.12% of the variance was explained by the first four principal components. Partial least squares discriminant analysis, naïve Bayes analysis, and back-propagation artificial neural network were used to develop the classification and prediction models. The 100% accuracy revealed a perfect classification of the botanical origins. In addition, the reliability and practicability of the models were validated by an independent set of additional 20 authentic honey samples. All 20 samples were accurately classified. The confidence measures indicated that the performance of the naïve Bayes model was better than the other two models. Finally, the characteristic volatile compounds of linden honey were tentatively identified. The proposed method is reliable and accurate for the classification of honey of various botanical origins.

Because of its unique characteristics of accurate mass full-spectrum acquisition, high resolution, and fast acquisition rates, GC-quadrupole-time-of-flight MS (GC-Q-TOF/MS) has become a powerful tool for pesticide residue analysis. In this study, a TOF accurate mass database and Q-TOF spectrum library of 439 pesticides were established, and the parameters of the TOF database were optimized. Through solid-phase extraction (SPE), whereby pesticides are extracted from fruit and vegetable substrates by using 40 mL 1% acetic acid in acetonitrile (v/v), purified by the Carbon/NH2 SPE cartridge, and finally detected by GC-Q-TOF/MS, the rapid analysis of 439 pesticides in fruits and vegetables can be achieved. The methodology verification results show that more than 70 and 91% of pesticides, spiked in fruits and vegetables with concentrations of 10 and 100 μg/kg, respectively, saw recoveries that conform to the European Commission's criterion of between 70 and 120% with RSD ≤20%. Eighty-one percent of pesticides have screening detection limits lower than 10 μg/kg, which makes this a reliable analysis technology for the monitoring of pesticide residues in fruits and vegetables. This technology was further validated for its characteristics of high precision, high speed, and high throughput through successful detection of 9817 samples during 2013-2015.

The performances of gas chromatography-tandem mass spectrometry (GC-MS/MS) and gas chromatography quadrupole time of flight mass spectrometry (GC-QTOF/MS) for the determination of 208 pesticide residues in fruit and vegetable samples, including apple, orange, tomato and cucumber, were compared comprehensively. Based on the differences of the two instruments, their respective characteristics and scopes of application in the detection of the pesticide residues were presented, which provided the reference for the analysis of pesticide residues. The performance parameters of the two instruments, such as overall recoveries, precisions, limits of detection, linear ranges, identification points and matrix effects, were evaluated according to a designed experiment. At three spiked levels (5.0, 10.0 and 20.0 µg/kg), the average recoveries for the majority of pesticides (93.0%) ranged from 70% to 120% in the four matrices with relative standard deviations below 20%. The limits of detection for most of the pesticides by GC-MS/MS and GC-Q-TOF/MS were less than 5.0 µg/kg. Compared with GC-QTOF/MS, GC-MS/MS showed relatively lower limits of detection and wider linear ranges, and its performance was more satisfactory in accurate quantitative analysis due to its superior sensitivity. On the other hand, GC-QTOF/MS provided accurate mass measurement, which was proved to be an efficient analytical tool on the rapid screening and confirmation of a large number of pesticides and non-target compounds.

By adding Fe3+ into an HCl carrier, thimerosal can be transformed into elemental mercury cold vapor in the presence of KBH4 and detected by AFS.