Bee Product Quality Supervision and Testing Center

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Bee Product Quality Supervision and Testing Center

Quality, China

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Zhou J.,Chinese Academy of Agricultural Sciences | Zhou J.,Bee Product Quality Supervision and Testing Center | Zhou J.,Laboratory of Risk Assessment for Quality and Safety of Bee Products | Qi Y.,Texas Heart Institute | And 11 more authors.
Food Research International | Year: 2014

We report the use of ultra performance liquid chromatography (UPLC) separation together with evaporative light scattering detection (ELSD) to effectively distinguish honey adulterated with maltooligosaccharides. UPLC separation utilizing a mobile phase with pure water and acetonitrile containing 0.2% triethylamine, resulted in enhanced separation and a running time of less than 6min. Also, only a simple liquid-liquid extraction was required for the sample pretreatment. This UPLC-ELSD method provides limits of quantifications (LOQs) from 0.30 to 0.60mg/g for the six maltooligosaccharides (maltose, maltotriose, maltotetraose, maltopentaose, maltohexaose and maltoheptaose) ranging from 15 to 2000μg/mL with excellent linearity(R2≥0.9914). This optimized method also offers a satisfactory intra-day precision of 2.4%-9.4%, inter-day precision of 5.5%-12.1% and accuracy of -7.7%-+11.4% at each level. We successfully applied this system for detecting maltooligosaccharide contamination in 290 honey samples collected from apiaries, supermarkets and traditional agri-product markets. Concentrations of the six maltooligosaccharides varied from undetectable to 14.1mg/mL. The lowest quantifiable concentration that could be detected by this established method was 0.132mg/mL. This study therefore demonstrates the reliability and potential use of the UPLC-ELSD technique in scrutinizing the authenticity of honey in the food processing industry. © 2014 Elsevier Ltd.


Zhou J.,Chinese Academy of Agricultural Sciences | Zhou J.,Bee Product Quality Supervision and Testing Center | Zhou J.,Laboratory of Risk Assessment for Quality and Safety of Bee Products | Yao L.,CAS South China Botanical Garden | And 12 more authors.
Food Chemistry | Year: 2014

A high performance liquid chromatography-diode array detection-tandem mass spectrometry (HPLC-DAD-MS/MS) method for the floral origin traceability of chaste honey and rape honey samples was firstly presented in this study. Kaempferol, morin and ferulic acid were used as floral markers to distinguish chaste honey from rape honey. Chromatographic fingerprinting at 270 nm and 360 nm could be used to characterise chaste honey and rape honey according to the analytical profiles. Principal component analysis (PCA), partial least squares (PLS), partial least squares-discrimination analysis (PLS-DA) and soft independent modeling of class analogy (SIMCA) were applied to classify the honey samples according to their floral origins. The results showed that chaste honey and rape honey could be successfully classified by their floral sources with the analytical methods developed through this study and could be considered encouraging and promising for the honey traceability from unifloral or multifloral nectariferous sources. © 2013 Elsevier Ltd. All rights reserved.


Xue X.,Chinese Academy of Agricultural Sciences | Xue X.,Risk Assessment Laboratory for Bee Products Quality | Xue X.,China Agricultural University | Wang Q.,Chinese Academy of Agricultural Sciences | And 5 more authors.
Journal of Agricultural and Food Chemistry | Year: 2013

The determination of honey authenticity is of importance to ensure its quality and safety. There is an urgent need of effective methods to detect adulterated honey. A simple, rapid, and effective HPLC-DAD method was developed to detect honey adulteration by rice syrup, using a characteristic compound from rice syrup, which is presently difficult to detect by current analytical methods. The characteristic compound was identified as 2-acetylfuran-3- glucopyranoside (AFGP) by MS and NMR. Based on HPLC analyses, the average concentration of AFGP was 92 ± 60 mg/kg in rice syrup. However, AFGP was not detected in any of the natural honey samples, so it could be used as a marker for the detection of honey adulteration by rice syrup. The developed method enabled a rapid detection of honey samples adulterated with 10% rice syrup. Using the developed method, 16 out of 186 honey samples from some markets were found to be adulterated with rice syrup. © 2013 American Chemical Society.


Zhou J.,Chinese Academy of Agricultural Sciences | Zhou J.,Bee Product Quality Supervision and Testing Center | Zhou J.,Apicultural Branch Center | Xu X.,Chinese Academy of Agricultural Sciences | And 7 more authors.
Analytical Methods | Year: 2012

An improved HPLC method was developed for the simultaneous determination of nucleosides in bee pollen samples of various floral origins. Bee pollen samples were dissolved in 35 mL pure water by agitation on a vortex mixer followed by ultrasonic-assisted extraction prior to quantitative analysis. HPLC conditions were optimized and good linearity (r 2 > 0.999) was obtained over the investigated concentration ranges. Precision was evaluated by intra- and inter-day assays and RSD values were below 3.15%. Accuracies ranged from 82.7% to 124.7%, respectively. Finally, the method was successfully applied to the analysis of nucleosides in bee pollen samples and could be used for routine analysis as the standard method. © 2012 The Royal Society of Chemistry.


Wu Z.-B.,Chinese Academy of Agricultural Sciences | Wu Z.-B.,Bee Product Quality Supervision and Testing Center | Chen F.,Chinese Academy of Agricultural Sciences | Chen F.,Laboratory of Quality and Safety Risk Assessment for Bee Products Beijing | And 13 more authors.
Guang Pu Xue Yu Guang Pu Fen Xi/Spectroscopy and Spectral Analysis | Year: 2015

In order to identify honeys according to their floral origin, inductively coupled plasma mass spectrometry (ICP-MS) combined with principal component analysis (PCA) and discriminant analysis (DA) were employed in the present study. Three kinds of honeys such as acacia honey samples, sunflower honey samples and rape honey samples were selected. It was pretreated by wet-acid digestionand measured 20 kinds of mineral elements in honey samples by ICP-MS. The result showed that the accuracy of the inductively coupled plasma mass spectrometrymeted the requirements. The result of principal component analysis demonstrated that the acacia honey samples were performed a trend of certain gather. The trend of the sunflower honey samples and the rape honey samples are not obvious. Ten kinds of mineral elements including Na, Mg, K, Ca, Sr, Ba, V, Fe, Ni, Sb can be regarded as honey varieties of characteristic elements. Seven kinds of mineral elements such as Mg, Sr, Ba, Sb, Ni, Cr and Na could be selected through stepwise discriminant analysis. Using bayes discriminant analysis, A linear discriminant function can be recieved. The discrimination rate of honey samples such as acacia honey samples, sunflower samples and rape honey samples were 100%, 80% and 90.9% respectively. Two sunflower honey samples was misclassified into rape honey samples andone rape honey samples are also misclassified into acacia honey sample. The total rate of discriminant model cross validation was 90.3%. It is concluded that the mineral elements in honey varieties with good classification. The present study can provide theoretical basis and the relationship between thetypes ofhoney samples with mineral elements. The method what this study used had simple, accurate and stablecharacteristics, which can be used as a reliable method of honey sample identification. ©, 2015, Science Press. All right reserved.


Zhang Y.-N.,Chinese Academy of Agricultural Sciences | Zhang Y.-N.,Risk Assessment Laboratory for Bee Products Quality and Safety of Ministry of Agriculture | Chen L.-Z.,Chinese Academy of Agricultural Sciences | Chen L.-Z.,Risk Assessment Laboratory for Bee Products Quality and Safety of Ministry of Agriculture | And 9 more authors.
Guang Pu Xue Yu Guang Pu Fen Xi/Spectroscopy and Spectral Analysis | Year: 2015

At present, the rice syrup as a low price of the sweeteners was often adulterated into acacia honey and the adulterated honeys were sold in honey markets, while there is no suitable and fast method to identify honey adulterated with rice syrup. In this study, Near infrared spectroscopy (NIR) combined with chemometric methods were used to discriminate authenticity of honey. 20 unprocessed acacia honey samples from the different honey producing areas, mixed?with different proportion of rice syrup, were prepared of seven different concentration gradient?including 121 samples. The near infrared spectrum (NIR) instrument and spectrum processing software have been applied in the?spectrum?scanning and data conversion on adulterant samples, respectively. Then it was analyzed by Principal component analysis (PCA) and canonical discriminant analysis methods in order to discriminating adulterated honey, The results showed that after principal components analysis, the first two principal components accounted for 97.23% of total variation, but the regionalism of the score plot of the first two PCs was not obvious, so the canonical discriminant analysis was used to make the further discrimination, all samples had been discriminated correctly, the first two discriminant functions accounted for 91.6% among the six canonical discriminant functions, Then the different concentration of adulterant samples can be discriminated correctly, it illustrate that canonical discriminant analysis method combined with NIR spectroscopy is not only feasible but also practical for rapid and effective discriminate of the rice syrup adulterant of acacia honey. © 2015, Science Press. All right reserved.


Zhou J.,Chinese Academy of Agricultural Sciences | Zhou J.,Bee Product Quality Supervision and Testing Center | Zhou J.,Laboratory of Risk Assessment for Quality and Safety of Bee Products | Qi Y.,Texas Heart Institute | And 5 more authors.
Journal of Separation Science | Year: 2014

A simple, rapid, and reliable liquid-liquid extraction coupled to GC-MS method was developed and validated for the quantification of 22 phthalate esters (PAEs) in honey and royal jelly. Instrument parameters for GC-MS were tested to obtain the satisfactory separation between 22 PAEs with high sensitivity. The extraction procedure was optimized in order to achieve the best recovery. The following criteria were used to validate the developed method: linearity, LOD, lower LOQ, precision, accuracy, matrix effect and carry-over. Correlation coefficients were >0.999 by applying the linear regression model based on the least-squares method with a weighting factor (1/x). The intra- and interday precision were within 12.7% in terms of RSD, and the accuracy was within -11.8% in terms of relative error. The mean extraction recoveries ranged between 80.1 and 110.9% for honey and royal jelly. No significant matrix effect and carry-over for PAEs were observed for the analysis of honey and royal jelly samples. A total of 20 real samples were analyzed for a mini-survey using the developed method. Seven PAEs in honey samples and five PAEs in royal jelly samples were found, indicating potential contamination with several PAEs. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.


Zhou J.,Chinese Academy of Agricultural Sciences | Zhou J.,Bee Product Quality Supervision and Testing Center | Zhou J.,Laboratory of Risk Assessment for Quality and Safety of Bee Products | Qi Y.,Texas Heart Institute | And 11 more authors.
Food Control | Year: 2015

The aim of this study was to develop and validate a method for reliable discrimination of bee pollen from different floral origins via simultaneous analysis of three flavonoid glycosides. A simple sample preparation procedure consisted of an ultrasonic-assisted extraction followed by high performance liquid chromatography-electrospray ionization-tandemmass spectrometry (HPLC-ESI-MS/MS) technique to effectively identify and differentiate ten kinds of bee pollens has been developed and optimized in this study. For sample extraction, several parameters were optimized including extraction solvents, extraction patterns, solvent volume, extraction duration and temperature. The analytical method was validated in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ), precision, matrix effect and carryover test using quality control sample. This method can consistently distinguish bee pollen by analyzing three flavonoid glycosides (quercetin-3-O-β- d-glucosyl-(2→l)-β-glucoside, kaempferol-3, 4'-di-O-β- d-glucoside and kaempferol-3-O-β- d-glucosyl-(2→l)-β- d-glucoside). Therefore, this technique will be a suitable to be used as a discrimination method to identify the floral origin of bee pollen via the proposed marker components. © 2015 Elsevier Ltd.


Li Y.,Chinese Academy of Agricultural Sciences | Li Y.,Bee Product Quality Supervision and Testing Center | Li Y.,Laboratory of Risk Assessment for Quality and Safety of Bee Products | Zhang J.,Chinese Academy of Agricultural Sciences | And 18 more authors.
Journal of Chromatography A | Year: 2016

This study reports a rapid, automated screening and quantification method for the determination of multi-xenobiotic residues in honey using ultra-high performance liquid chromatography-hybrid quadrupole-Orbitrap mass spectrometry (UHPLC-Q-Orbitrap) with a user-built accurate-mass database plus parallel reaction monitoring (PRM). The database contains multi-xenobiotic information including formulas, adduct types, theoretical exact mass and retention time, characteristic fragment ions, ion ratios, and mass accuracies. A simple sample preparation method was developed to reduce xenobiotic loss in the honey samples. The screening method was validated based on retention time deviation, mass accuracy via full scan-data-dependent MS/MS (full scan-ddMS2), multi-isotope ratio, characteristic ion ratio, sensitivity, and positive/negative switching performance between the spiked sample and corresponding standard solution. The quantification method based on the PRM mode is a promising new quantitative tool which we validated in terms of selectivity, linearity, recovery (accuracy), repeatability (precision), decision limit (CCα), detection capability (CCβ), matrix effects, and carry-over. The optimized methods proposed in this study enable the automated screening and quantification of 157 compounds in less than 15. min in honey. The results of this study, as they represent a convenient protocol for large-scale screening and quantification, also provide a research approach for analysis of various contaminants in other matrices. © 2015 Elsevier B.V..


Li Y.,Chinese Academy of Agricultural Sciences | Li Y.,Bee Product Quality Supervision and Testing Center | Li Y.,Laboratory of Risk Assessment for Quality and Safety of Bee Products | Qi Y.,Texas Heart Institute | And 8 more authors.
Natural Product Research | Year: 2016

To identify the structures of flavonoid glycosides in bee pollen collected from rapeseed plants (Brassica napus L.), we utilised an approach that combined liquid chromatography-diode array detector-electrospray ionization-mass spectrometry (LC-DAD-ESI-MS) and nuclear magnetic resonance (NMR) technology with a step-wise separation strategy. We identified four constituents of high purity in rape bee pollen samples: (1) quercetin-3-O-β-D-glucosyl-(2→l)-β-glucoside, (2) kaempferol-3, 4'-di-O-β-D-glucoside, (3) 5, 7, 4'-trihydroxy-3'-methoxyflavone-3-O-β-D-sophoroside and (4) kaempferol-3-O-β-D-glucosyl-(2→l)-β-D-glucoside. This study will also provide useful reference standards for qualification and quantification of four flavonoid glycosides in natural products. © 2015 Taylor & Francis.

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