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1.
Fourier transform infrared spectroscopy and attenuated total reflection sampling have been used to detect adulteration of single strength apple juice samples. The sample set comprised 224 authentic apple juices and 480 adulterated samples. Adulterants used included partially inverted cane syrup (PICS), beet sucrose (BS), high fructose corn syrup (HFCS), and a synthetic solution of fructose, glucose, and sucrose (FGS). Adulteration was carried out on individual apple juice samples at levels of 10, 20, 30, and 40% w/w. Spectral data were compressed by principal component analysis and analyzed using k-nearest neighbors and partial least squares regression techniques. Prediction results for the best classification models achieved an overall (authentic plus adulterated) correct classification rate of 96.5, 93.9, 92.2, and 82.4% for PICS, BS, HFCS, and FGS adulterants, respectively. This method shows promise as a rapid screening technique for the detection of a broad range of potential adulterants in apple juice.  相似文献   

2.
Fourier transform infrared (FTIR) spectroscopy and attenuated total reflection (ATR) sampling have been used to detect adulteration of honey samples. The sample set comprised 320 spectra of authentic (n = 99) and adulterated (n = 221) honeys. Adulterants used were solutions containing both d-fructose and d-glucose prepared in the following respective weight ratios: 0.7:1.0, 1.2:1.0 (typical of honey composition), and 2.3:1.0. Each adulterant solution was added to individual honeys at levels of 7, 14, and 21% w/w. Spectral data were compressed and analyzed using k-nearest neighbors (kNN) and partial least squares (PLS) regression techniques. A number of data pretreatments were explored. Best classification models were achieved with PLS regression on first derivative spectra giving an overall correct classification rate of 93%, with 99% of samples adulterated at levels of 14% w/w or greater correctly identified. This method shows promise as a rapid screening technique for detection of this type of honey adulteration.  相似文献   

3.
Honey adulterations can be carried out by addition of inexpensive sugar syrups, such as high fructose corn syrup (HFCS) and inverted syrup (IS). Carbohydrate composition of 20 honey samples (16 nectar and 4 honeydew honeys) and 6 syrups has been studied by GC and GC-MS in order to detect differences between both sample groups. The presence of difructose anhydrides (DFAs) in these syrups is described for the first time in this paper; their proportions were dependent on the syrup type considered. As these compounds were not detected in any of the 20 honey samples analyzed, their presence in honey is proposed as a marker of adulteration. Detection of honey adulteration with HFCS and IS requires a previous enrichment step to remove major sugars (monosaccharides) and to preconcentrate DFAs. A new methodology based on yeast (Saccharomyces cerevisiae) treatment has been developed to allow the detection of DFAs in adulterated honeys in concentrations as low as 5% (w/w).  相似文献   

4.
A new procedure to determine individual sugar (sucrose, glucose, and fructose) 13C isotope ratios, using liquid chromatography-isotope ratio mass spectrometry (HPLC-IRMS), has been developed to improve isotopic methods devoted to the study of honey authenticity. For this purpose 79 commercial honey samples from various origins were analyzed. Values of delta13Choney ranged from -14.2 to -27.2", and delta13Cprotein ranged from -23.6 to -26.9". A very strong correlation is observed between the individual sugar 13C ratios, which are altered in the event of sugar addition, even at low levels. The use of Deltadelta13C [fruct-glu], Deltadelta13C [fruct-suc], and Deltadelta13C [gluc-suc] systematic differences as an authenticity criterion permits the sugar addition [C3, beet sugar; or C4, cane sugar, cane syrup, isoglucose syrup, and high-fructose corn syrup (HFCS)] to be reliably detected (DL = 1-10%). The new procedure has advantages over existing methods in terms of analysis time and sensitivity. In addition, it is the first isotopic method developed that allows beet sugar addition detection.  相似文献   

5.
基于近红外光谱技术的蜂蜜掺假识别   总被引：7，自引：1，他引：6  
为了实现蜂蜜掺假的快速识别,应用近红外光谱结合模式识别方法对蜂蜜掺假现象进行了识别分析。该研究收集了中国不同品种、不同地域的典型天然蜂蜜样品,根据目前市场上常见的蜂蜜掺假手段,掺假物质及相对含量情况配制了掺假蜂蜜样品,利用傅立叶近红外光谱仪采集其透反射近红外光谱,分别采用偏最小二乘判别分析（PLS-DA）,独立软模式法（SIMCA）,误差反向传播神经网络（BP-ANN）和最小二乘支持向量机（LS-SVM）等模式识别方法,进行蜂蜜掺假识别研究。研究结果表明：利用这4种方法在蜂蜜中掺入果葡糖浆和果葡糖水的情况下均能很好地识别出掺假蜂蜜样品,其中对于掺入果葡糖浆的掺假情况,校正集的正确判别率均达到95%以上,验证集的正确判别率均达到87%以上,对于掺入果葡糖水的掺假蜂蜜校正集的正确判别率均达到93%以上,验证集的正确判别率均达到84%以上。通过比较4种不同的识别算法,发现采用LS-SVM时,对两种掺假情况下校正集和验证集的正确判别率均达到了100%,表明基于近红外光谱的蜂蜜掺假快速准确识别是可行的。  相似文献   

6.
A gas-liquid chromatographic (GLC) method has been developed to detect the addition to honey of high fructose corn sirup (HFCS). Samples are derivatized directly with trimethylsilane, cholestane is added as an internal standard, and the levels of maltose (includes other minor disaccharides) and isomaltose are determined after chromatography on OV-17. Domestic and imported honey samples (115) contained 2.00% maltose and 0.71% isomaltose. HFCS samples (21) contained 1.50% maltose, and 2.09% isomaltose. A discriminatory equation was developed (D = 2.73 - 5. 35 (Isomaltose/maltose)) and, when applied to the data for these samples and 37 adulterated samples, 81.4% of authentic honey samples and 78.4% of samples known to be adulterated with HFCS were correctly classified.  相似文献   

7.
Stable carbon isotope ratio mass spectrometry (delta13C IRMS) was used to detect maple syrup adulteration by exogenous sugar addition (beet and cane sugar). Malic acid present in maple syrup is proposed as an isotopic internal standard to improve actual adulteration detection levels. A lead precipitation method has been modified to isolate quantitatively malic acid from maple syrup using preparative reversed-phase liquid chromatography. The stable carbon isotopic ratio of malic acid isolated from this procedure shows an excellent accuracy and repeatability of 0.01 and 0.1 per thousand respectively, confirming that the modified lead precipitation method is an isotopic fractionation-free process. A new approach is proposed to detect adulteration based on the correlation existing between the delta13Cmalic acid and the delta13Csugars-delta13Cmalic acid (r = 0.704). This technique has been tested on a set of 56 authentic maple syrup samples. Additionally, authentic samples were spiked with exogeneous sugars. The mean theoretical detection level was statistically lowered using this technique in comparison with the usual two-standard deviation approach, especially when maple syrup is adulterated with beet sugar : 24 +/- 12% of adulteration detection versus 48 +/- 20% (t-test, p = 7.3 x 10-15). The method was also applied to published data for pineapple juices and honey with the same improvement.  相似文献   

8.
Differential scanning calorimetry (DSC) was used to study the thermal behavior of authentic honeys (Lavandula, Robinia, and Fir honeys) and industrial sugar syrups. Thermal or thermochemical parameters such as the glass transition temperature (Tg), enthalpies of fusion (DeltaH(fus)), and heat capacity variation (DeltaC(p)) were measured. The syrups and honeys showed significant differences in thermal phenomena, as well as in their amplitude and position on the temperature scale. Results showed good reproducibility of the method for all samples studied. The effect of adulteration of honey with different amounts of syrup (5, 10, 20, 40, and 60%) was investigated. A linear relationship was found between the percentage of added syrup and the glass transition temperature. A similar relationship was obtained from the enthalpy of fusion results in the temperature range of 40-90 degrees C. Under applied conditions, the effects of adulteration of honeys by industrial syrups appeared to be detectable from a level as low as 5%.  相似文献   

9.
NIR transflectance spectroscopy was used to determine polarimetric parameters (direct polarization, polarization after inversion, specific rotation in dry matter, and polarization due to nonmonosaccharides) and sucrose in honey. In total, 156 honey samples were collected during 1992 (45 samples), 1995 (56 samples), and 1996 (55 samples). Samples were analyzed by NIR spectroscopy and polarimetric methods. Calibration (118 samples) and validation (38 samples) sets were made up; honeys from the three years were included in both sets. Calibrations were performed by modified partial least-squares regression and scatter correction by standard normal variation and detrend methods. For direct polarization, polarization after inversion, specific rotation in dry matter, and polarization due to nonmonosaccharides, good statistics (bias, SEV, and R(2)) were obtained for the validation set, and no statistically (p = 0.05) significant differences were found between instrumental and polarimetric methods for these parameters. Statistical data for sucrose were not as good as those of the other parameters. Therefore, NIR spectroscopy is not an effective method for quantitative analysis of sucrose in these honey samples. However, NIR spectroscopy may be an acceptable method for semiquantitative evaluation of sucrose for honeys, such as those in our study, containing up to 3% of sucrose. Further work is necessary to validate the uncertainty at higher levels.  相似文献   

10.
A highly sensitive procedure has been developed to detect the undeclared addition of high fructose corn sirup (HFCS) to honey. Carbohydrates must be separated first to achieve the requisite degree of sensitivity; charcoal-Celite chromatography was used to isolate a fraction containing oligo- and polysaccharides. The fraction was then concentrated and examined by thin layer chromatography on silica gel. Pure honeys yielded only 1 or 2 blue-grey or blue-brown spots at Rf values greater than 0.35; a series of spots or blue streaks extending from the origin characterized adulterated samples. The method detects HFCS and conventional honey adulterants at levels as low as 10% or less of the total mixture. In addition, the procedure detects the presence in honey of all starch-derived sugar sirups tested thus far, regardless of the plant source.  相似文献   

11.
Fourier transform near-infrared spectroscopy (FT-NIR) was evaluated for the authentication of eight unifloral and polyfloral honey types (n = 364 samples) previously classified using traditional methods such as chemical, pollen, and sensory analysis. Chemometric evaluation of the spectra was carried out by applying principal component analysis and linear discriminant analysis. The corresponding error rates were calculated according to Bayes' theorem. NIR spectroscopy enabled a reliable discrimination of acacia, chestnut, and fir honeydew honey from the other unifloral and polyfloral honey types studied. The error rates ranged from <0.1 to 6.3% depending on the honey type. NIR proved also to be useful for the classification of blossom and honeydew honeys. The results demonstrate that near-infrared spectrometry is a valuable, rapid, and nondestructive tool for the authentication of the above-mentioned honeys, but not for all varieties studied.  相似文献   

12.
The potential of Fourier transform mid-infrared spectroscopy (FT-MIR) using an attenuated total reflectance (ATR) cell was evaluated for the authentication of 11 unifloral (acacia, alpine rose, chestnut, dandelion, heather, lime, rape, fir honeydew, metcalfa honeydew, oak honeydew) and polyfloral honey types (n = 411 samples) previously classified with traditional methods such as chemical, pollen, and sensory analysis. Chemometric evaluation of the spectra was carried out by applying principal component analysis and linear discriminant analysis, the error rates of the discriminant models being calculated by using Bayes' theorem. The error rates ranged from <0.1% (polyfloral and heather honeys as well as honeydew honeys from metcalfa, oak, and fir) to 8.3% (alpine rose honey) in both jackknife classification and validation, depending on the honey type considered. This study indicates that ATR-MIR spectroscopy is a valuable tool for the authentication of the botanical origin and quality control and may also be useful for the determination of the geographical origin of honey.  相似文献   

13.
Isotope parameters (δ(13)C(honey), δ(13)C(protein), δ(15)N) were determined for 271 honey samples of 7 types (black locust, multifloral, lime, chestnut, forest, spruce, and fir honeys) from 4 natural geographical regions of Slovenia. Carbon and nitrogen stable isotope ratios were measured to elucidate the applicability of this method in the identification of the botanical and geographical origin of honey and in honey adulteration. Only 2.2% of the samples were adulterated according to the internal standard carbon isotope ratio analysis method. Botanical origin did not have any major influence on the honey isotope profiles; only black locust honey showed higher δ(13)C values. Some differences were seen across different production years, indicating that the influence of season should be further tested. Statistical and multivariate analyses demonstrated differences among honeys of various geographical origins. Those from the Alpine region had low δ(13)C (-26.0‰) and δ(15)N values (1.1‰); those from the Mediterranean region, high δ(13)C (-24.6‰) and medium δ(15)N values (2.2‰); those from the Pannonian region, medium δ(13)C (-25.6‰) and high δ(15)N value (3.0‰); and those from the Dinaric region, medium δ(13)C (-25.7‰) and low δ(15)N values (1.4‰).  相似文献   

14.
Front-face fluorescence spectroscopy, directly applied on honey samples, was used for the authentication of 11 unifloral and polyfloral honey types (n = 371 samples) previously classified using traditional methods such as chemical, pollen, and sensory analysis. Excitation spectra (220-400 nm) were recorded with the emission measured at 420 nm. In addition, emission spectra were recorded between 290 and 500 nm (excitation at 270 nm) as well as between 330 and 550 nm (excitation at 310 nm). A total of four different spectral data sets were considered for data analysis. Chemometric evaluation of the spectra included principal component analysis and linear discriminant analysis; the error rates of the discriminant models were calculated by using Bayes' theorem. They ranged from <0.1% (polyfloral and chestnut honeys) to 9.9% (fir honeydew honey) by using single spectral data sets and from <0.1% (metcalfa honeydew, polyfloral, and chestnut honeys) to 7.5% (lime honey) by combining two data sets. This study indicates that front-face fluorescence spectroscopy is a promising technique for the authentication of the botanical origin of honey and may also be useful for the determination of the geographical origin within the same unifloral honey type.  相似文献   

15.
Fourier transform infrared spectroscopy (FTIR) and z-Nose were used as screening tools for the identification and classification of honey from different floral sources. Honey samples were scanned using microattenuated total reflectance spectroscopy in the region of 600-4000 cm(-1). Spectral data were analyzed by principal component analysis, canonical variate analysis, and artificial neural network for classification of the different honey samples from a range of floral sources. Classification accuracy near 100% was achieved for clover (South Dakota), buckwheat (Missouri), basswood (New York), wildflower (Pennsylvania), orange blossom (California), carrot (Louisiana), and alfalfa (California) honey. The same honey samples were also analyzed using a surface acoustic wave based z-Nose technology via a chromatogram and a spectral approach, corrected for time shift and baseline shifts. On the basis of the volatile components of honey, the seven different floral honeys previously mentioned were successfully discriminated using the z-Nose approach. Classification models for FTIR and z-Nose were successfully validated (near 100% correct classification) using 20 samples of unknown honey from various floral sources. The developed FTIR and z-Nose methods were able to detect the floral origin of the seven different honey samples within 2-3 min based on the developed calibrations.  相似文献   

16.
HPLC-DAD-MS/MS chromatograms of thistle (Galactites tomentosa Moench) unifloral honeys, previously selected by sensory evaluation and melissopalynological analysis, showed high levels of two compounds. One was characterized as phenyllactic acid, a common acid found in honeys, but the other compound was very unusual for honeys. This compound was extracted from honey with ethyl acetate and purified by SPE using C(18), SiOH, and NH(2) phases. Its structure was elucidated on the basis of extensive 1D and 2D NMR experiments as well as HPLC-MS/MS and Q-TOF analysis, and it was identified as lumichrome (7,8-dimethylalloxazine). Lumichrome is known to be the main product of degradation obtained in acid medium from riboflavin (vitamin B(2)), and this is the first report of the presence of lumichrome in honeys. Analysis of the G. tomentosa raw honey and flowers extracts confirmed the floral origin of this compound. The average amount of lumichrome in thistle honey was 29.4 ± 14.9 mg/kg, while phenyllactic acid was 418.6 ± 168.9 mg/kg. Lumichrome, along with the unusual high level of phenyllactic acid, could be used as a marker for the botanical classification of unifloral thistle (G. tomentosa) honey.  相似文献   

17.
Using the difference in stable carbon isotope ratio between a honey and its protein fraction permits objective evaluation of possible adulteration of honey with small amounts (7-20%) as well as larger amounts of corn or cane sugar. The present uncertainty in interpretation of results from pure honey with delta 13C values outside the generally accepted limits for pure honey of -27.5% to -23.5% is eliminated; likewise TLC testing to resolve questionable samples with delta 13C values between -23.5 and -21.5% is not needed. Fifty certified samples of pure honey were used to establish criteria for purity, and 38 other samples with delta 13C values in the "questionable" or "adulterated" range for the AOAC official method were tested. A difference of 1.0% or more between honey and protein fractions is proposed to indicate adulteration.  相似文献   

18.
Thirteen metal elements were determined in 40 honey samples from Galicia with different environmental origins: rural, urban, and industrial areas. The data set of the honey metallic profiles was studied with a double purpose: first, to make a preliminary evaluation of honey as an environmental indicator in Galicia with the aim of monitoring pollution and, second, to compare the different capabilities of diverse pattern recognition prediction procedures for modeling the environmental surrounding of the hive. A certain level of similarity for urban and industrial samples was obtained using principal component analysis and cluster analysis, whereas significant differences for urban and industrial honeys were found in relation to rural honey samples. Different classification rules to associate metal content of honeys with their environmental surrounding were obtained by chemometric pattern recognition procedures. In general, the classification methods developed by neural networks provided better results than the traditional pattern recognition procedures. The metal profiles of honey seem to provide sufficient information to enable categorization criteria for classifying samples according to their environmental surrounding. Thus, honey could be a potential pollution indicator for the Galician area.  相似文献   

19.
The primary objective of this study was to determine how yogurt ingredients affect aroma release in the mouth during eating. A model strawberry flavor consisting of ethyl butanoate, ethyl 3-methylbutanoate, (Z)-hex-3-enol, 2-methylbutanoic acid, 5-hexylhydro-2(3H)-furanone, and 3-methyl-3-phenylglycidic acid ethyl ester was added to unflavored, unsweetened yogurt that had different added sweeteners and hydrocolloids. In all, 12 yogurt formulations were examined to determine the effects of gelatin, modified food starch, pectin, sucrose, high-fructose corn syrup, and aspartame on aroma release. Aroma release was monitored by breath-by-breath analysis (proton-transfer reaction-mass spectrometry) during eating of the test yogurts. Results showed aroma release of the ethyl butanoate, (Z)-hex-3-enol, and ethyl 3-methylbutanoate to be suppressed by sweeteners, with 55 DE high-fructose corn syrup having the greatest effect. Addition of thickening agents had no significant effect on the aroma release profiles of the compounds under study.  相似文献   

20.
Determination of changes in 2-furoylmethyl amino acids and hydroxymethylfurfural during the storage of four honey samples at 25 and 35 degrees C during 12 months was achieved to assess the potential use of both parameters, singly or in combination, as quality indicators. 2-Furoylmethyl amino acids increased during storage at both temperatures, whereas hydroxymethylfurfural only presented slight variations during storage at 25 degrees C but increased noticeably at 35 degrees C. The study of 2-furoylmethyl amino acids in 49 commercial honeys revealed that 2-furoylmethyl lysine (furosine) was present in all samples, whereas 2-furoylmethyl derivatives of arginine, GABA, and proline were only present in seven samples. Hydroxymethylfurfural can be considered as a good indicator of heat treatments applied to honey samples, whereas 2-furoylmethyl amino acids can be used as suitable markers of the storage period. The use of both parameters can be useful to detect adulteration with invert syrups, excessive heat treatments, or prolonged storage of honey samples.  相似文献   

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