Survey results of benzene in soft drinks and other beverages by headspace gas chromatography/mass spectrometry

Benzene, a carcinogen that can cause cancer in humans, may form at nanogram per gram levels in some beverages containing both benzoate salts and ascorbic or erythorbic acids. Through a series of reactions, a hydroxyl radical forms that can decarboxylate benzoate to form benzene. Elevated temperatures and light stimulate these reactions, while sugar and ethylenediaminetetraacetic acid (EDTA) can inhibit them. A headspace gas chromatography/mass spectrometry method for the determination of benzene in beverages was developed and validated. The method was used to conduct a survey of 199 soft drinks and other beverages. The vast majority of beverages sampled contained either no detectable benzene or levels below the U.S. Environmental Protection Agency's drinking water limit of 5 ng/g. Beverages found to contain 5 ng/g benzene or more were reformulated by the manufacturers. The amount of benzene found in the reformulated beverages ranged from none detected to 1.1 ng/g.     

Multielement analysis of soft drinks by X-ray fluorescence spectrometry

Several commercial soft drinks and respective plastic bottles were analyzed for their multielement contents employing the synchrotron radiation total reflection X-ray fluorescence spectrometry technique (SRTXRF). The SRTXRF method has been developed and validated, and about 20 elements were detected in the investigated samples, including some trace elements, which can be toxic for human beings, such as Ti, Cr, Sb, As, and Pb in soft drinks and Al, Sb, As, and Pb in poly(ethylene terephthalate) (PET) containers. Statistical analysis was performed using chemometric techniques (principal component analysis and cluster analysis), and similarities were verified in the multielement contents of the samples. The results demonstrated that the SRTXRF offers a good multielemental approach for the quality control of food products. Moreover, on the basis of enrichment factors, the possibility of the trace elements in the PET container may be leached to the beverages under normal commercial situations and other results were discussed.     

Authentication of the botanical and geographical origin of honey by mid-infrared spectroscopy

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.     

Detection of adulteration in cooked meat products by mid-infrared spectroscopy

Mid-infrared spectroscopy was used to discriminate between pure beef and beef containing 20% w/w of a range of potential adulterants (heart, tripe, kidney, and liver). Spectra were acquired from raw samples and from samples cooked using two different cooking regimes. Chemometric methods (principal component analysis, partial least squares regression, and linear discriminant analysis) applied to the spectra showed that discrimination between the pure and adulterated sample types was possible, irrespective of cooking regime. The cross-validated classification success rate obtained was approximately 97%. Discrimination between all five sample types (pure beef and beef containing one of each of the four adulterants) at each level of cook was also possible, but became more difficult as the cooking level increased.     

果汁和饮料中糖组分的超声检测研究

为研究果汁、饮料生产中糖浓度的在线快速测定技术,采用基于超声传播特性的液态食品质量检测装置,测定了纯果糖、葡萄糖、蔗糖溶液及葡萄糖—蔗糖混合溶液的糖组分浓度与声速的关系。结果表明：纯糖溶液中声速与浓度用二次方程回归呈极显著正相关(R²>0.9970);声速与混合溶液糖组分浓度关系密切,可用二元二次多项式拟合(P<0.0001);采用声速与浓度的经验公式和与理论结合的半经验公式组成方程组,对果汁饮料中的还原糖、蔗糖和总糖含量进行分析,与传统检测方法和高效液相色谱法(HPLC)的检测结果一致,其差异不显著(P≤0.05)。该研究表明超声检测技术有可能应用于果汁、饮料中糖组分浓度的检测。     

中红外光谱土壤有机质含量估测研究进展

中红外光谱波段(2.5～25μm)对土壤有机质内部分子振动高度敏感,基于中红外光谱技术的土壤有机质含量估测是土壤学科新兴的研究方向和热点.文章采用文献综述的方法,全面总结了土壤有机质含量中红外光谱估测方法的发展和应用,简述了中红外光谱响应与土壤有机质分子结构的相关性研究,对比分析了室内台式、手持式和机载中红外光谱设备估...     

Sensitive determination of sulfate in drinks and vegetables digests by Rayleigh light scattering technique

In this paper, a novel and sensitive method based on Rayleigh light scattering technique (RLS) was proposed for the determination of sulfate using a conventional spectrofluorometer. Sulfate was transformed to BaSO4 particles, which displayed intense light scattering in aqueous solutions. The effects of factors such as wavelength, acidity, stabilizers and interferents were studied in detail. The RLS intensity of the BaSO4 suspension was obtained in 0.1 mol L(-1) of [H+] and the addition of 2 mL of cationic polyacrylamide (CPAM) with 7.05 x 10(-3) mmol mL(-1) charged cations and 1.0 mL of BaCl2.2H2O (5.0%) at 510 nm. In the range of 8-400 microg mL(-1), RLS intensity was linear to the concentration of BaSO4, and the detection limit was 0.3 microg mL(-1). To determine the feasibility of the proposed method, some samples of water, drinks, and vegetables digests were analyzed, and the results were in agreement with the standard turbidimetric method. Good recovery results were also obtained in the range of 94-105%. Although this method was limited in stability, it was characterized with simplicity, sensitivity, reliability, and little interference.     

Quantitative ester analysis in cachaca and distilled spirits by gas chromatography-mass spectrometry (GC-MS)

An analytical procedure for the separation and quantification of ethyl acetate, ethyl butyrate, ethyl hexanoate, ethyl lactate, ethyl octanoate, ethyl nonanoate, ethyl decanoate, isoamyl octanoate, and ethyl laurate in cachaca, rum, and whisky by direct injection gas chromatography-mass spectrometry was developed. The analytical method is simple, selective, and appropriated for the determination of esters in distilled spirits. The limit of detection ranged from 29 (ethyl hexanoate) to 530 (ethyl acetate) microg L(-1), whereas the standard deviation for repeatability was between 0.774% (ethyl hexanoate) and 5.05% (isoamyl octanoate). Relative standard deviation values for accuracy vary from 90.3 to 98.5% for ethyl butyrate and ethyl acetate, respectively. Ethyl acetate was shown to be the major ester in cachaca (median content of 22.6 mg 100 mL(-1) anhydrous alcohol), followed by ethyl lactate (median content of 8.32 mg 100 mL(-1) anhydrous alcohol). Cachaca produced in copper and hybrid alembic present a higher content of ethyl acetate and ethyl lactate than those produced in a stainless-steel column, whereas cachaca produced by distillation in a stainless-steel column present a higher content of ethyl octanoate, ethyl decanoate, and ethyl laurate. As expected, ethyl acetate is the major ester in whiskey and rum, followed by ethyl lactate for samples of rum. Nevertheless, whiskey samples exhibit ethyl lactate at contents lower or at the same order of magnitude of the fatty esters.     

近红外光谱联合CARS-PLS-LDA的山茶油检测

为了寻找快速判别山茶油掺假的检测方法,本研究利用近红外光谱技术对掺杂大豆没油山茶油进行掺假检测研究.试验在350～1 800 nm波段范围内采集样本的透射光谱,利用CARS方法筛选重要的波长变量,应用偏最小二乘-线性判别分析(PLS-LDA)建立山茶油掺假的判别模型,并与未经变量优选的判别模型进行比较.结果表明,近红外光谱技术联合CARS-PLS-LDA方法可以有效判别纯山茶油和掺假山茶油,校正集、预测集及独立样本组样本的判别正确率、灵敏度及特异性均为100％.CARS-PLS-LDA判别模型性能优于未经变量优选的判别模型,表明CARS方法可以有效筛选重要波长变量,能简化判别模型及提高判别模型的稳定性和判别精度.本研究可为山茶油掺假快速检测提供理论依据.     

Development of a rapid "fingerprinting" system for wine authenticity by mid-infrared spectroscopy

This paper reports on the development of a rapid and simple method for red wine authenticity confirmation during transport and processing; namely, a wine "fingerprinting" system. When wine is transported between two sites, a sample is taken and a mid-infrared (MIR) spectrum is obtained. One hundred sixty-one (n = 161) samples of three main red wine varieties grown in Australia, Shiraz, Cabernet Sauvignon, and Merlot, were collected from six commercial wineries across Australia and scanned in transmission on two MIR spectrophotometers located at The Hardy Wine Company's main site at Reynella, South Australia (Foss WineScan FT 120) (926-5012 cm-1). A similarity index (SI) method was used as a tool to classify wine samples on the basis of their spectral data. The results showed that high rates of classification were obtained when wine samples scanned in different instruments were analyzed. The SI has been proven to provide an acceptable measurement for authentication of red wine integrity during transportation. In five of the six winery data sets, the SI correctly classified 98% of the wines. It was also observed that less than 1% of wines were misclassified between the different wineries investigated. Further studies are needed in order to test the applicability of the SI in a commercial situation and to evaluate its potential as a rapid quality control tool for routine use to authenticate wine samples during transport.     

Prediction of relative tissue proportions in wheat mill streams by fourier transform mid-infrared spectroscopy

Fourier-transform mid-infrared (FTIR) spectroscopy was investigated as a method to quantify the relative wheat grain tissue proportion in milling fractions. Spectra were acquired with a FTIR spectrometer equipped with an attenuated total reflectance device on ground samples, and the relative tissue proportion was determined according to the biochemical marker methodology as the reference method. Partial least-squares models were developed independently to predict the amount of outer pericarp, aleurone layer, starchy endosperm, and an intermediate layer (made up of inner pericarp plus seed coat plus nucellar epidermis). Good quality of prediction was obtained regardless of the target tissue. The standard errors of prediction obtained for the outer pericarp, intermediate layer, aleurone layer, and starchy endosperm quantification were, respectively, 3.4, 1.3, 3.4, and 4.6%.     

Classification of smoke tainted wines using mid-infrared spectroscopy and chemometrics

In this study, the suitability of mid-infrared (MIR) spectroscopy, combined with principal component analysis (PCA) and linear discriminant analysis (LDA), was evaluated as a rapid analytical technique to identify smoke tainted wines. Control (i.e., unsmoked) and smoke-affected wines (260 in total) from experimental and commercial sources were analyzed by MIR spectroscopy and chemometrics. The concentrations of guaiacol and 4-methylguaiacol were also determined using gas chromatography-mass spectrometry (GC-MS), as markers of smoke taint. LDA models correctly classified 61% of control wines and 70% of smoke-affected wines. Classification rates were found to be influenced by the extent of smoke taint (based on GC-MS and informal sensory assessment), as well as qualitative differences in wine composition due to grape variety and oak maturation. Overall, the potential application of MIR spectroscopy combined with chemometrics as a rapid analytical technique for screening smoke-affected wines was demonstrated.     

Production and composition of cider spirits distilled in "alquitara"

The capacity of alquitara (a traditional distillation system) to produce cider brandies is evaluated. To do so, the chemical composition of 12 fractions obtained during the distillation process and the cider brandies obtained from five ciders were analyzed (alcohol strength, methanol, volatile substances, furfural, and metals), taking into account European and Spanish legislation. During the course of distillation, an important increase in methanol, furfural, 2-phenylethanol, and metals in the last fractions was observed, while fusel oils were more abundant in the first fractions collected. Only acetaldehyde behaved differently, showing a minimum concentration in the middle fractions that might be explained by its formation on the surface of alquitara. On the other hand, the final distillates obtained by means of this method complied with the considered regulations. Worth highlighting in this regard are the low levels of a potential toxin such as methanol, as well as the detection of a constant ratio for methanol, ethanol, and fusel oil for the pairs of cider/spirits analyzed, which could be interpreted as an indication of good uniformity in the distillation system and method, thus guaranteeing product quality.     

基于中红外光谱的规模化奶牛场粪水总氮快速预测方法

为建立适用于规模化奶牛场粪水中总氮含量的快速预测方法,以天津市23家种养结合型规模化奶牛场粪水治理全过程环节的样品为研究对象,探讨了基于中红外衰减全反射光谱技术快速预测粪水总氮含量的可行性。以偏最小二乘法分别建立了同一奶牛场粪水总氮含量的全程定标模型和不同奶牛场粪水总氮含量的全局定标模型,并采用独立的预测集验证了模型有效性。结果表明:全程模型总氮预测含量与实测含量的线性拟合相关系数为0.98,预测均方根误差RMSEP为130.18 mg/L,剩余预测偏差为4.97,可用于某一奶牛场粪水运移全过程环节总氮含量的快速预测;全局模型总氮预测含量与实测含量的线性拟合相关系数为0.97,预测均方根误差RMSEP为191.66 mg/L,剩余预测偏差为3.83,可用于不同奶牛场多元因素条件下总氮含量的快速预测。研究表明,基于中红外衰减全反射光谱可以实现对不同类型规模化奶牛场粪水治理全过程环节样品总氮含量的即时监测和跟踪。     

用偏最小二乘法及傅立叶变换近红外光谱快速检测白酒酒精度

为了得到白酒工业中酒精度的快速检测技术,将偏最小二乘法与傅立叶变换近红外光谱相结合,通过解析白酒样品的近红外光谱图和对光谱进行不同的预处理,结果表明：用最大最小归一化法预处理光谱,光谱范围选择9747.1～7498.3 cm^-1和6102～5446.3 cm^-1,采用内部交叉验证建立模型,决定系数(R²)为99.99%,交互验证均方根差(RMSECV)为0.165%,主成分数为4,此条件下建模效果较好;模型进行验证结果表明预测集相关系数(R²)为99.80%,预测标准偏差(RMSEP)为0.264%,模型的预测效果很好,具有较高的精密度和良好的稳定性,能满足生产中白酒酒精度的快速检测要求。     

Potentiometric flow injection determination of glycerol in distilled spirits.

A single-line flow injection system including a tubular periodate-selective electrode without inner reference solution is proposed for glycerol determination in distilled spirits, based on oxidation of this polyol by periodate. Interferences due to 5.0 mg L(-1) Cu, 5000 mg L(-1) sucrose, and 3000 mg L(-1) fructose plus glucose were investigated. The procedure is characterized by a linear response for 20-500 mg L(-1) glycerol (r > 0.9999, n = 7), a relative standard deviation of results of <0.03, and an analytical throughput of 30 determinations per hour. Accuracy was assessed by applying the procedure to distilled spirits of sugarcane and grape already analyzed by HPLC; in addition, recoveries within 96 and 120% were obtained.     

Degradation of green tea catechins in tea drinks

Green tea cateachins (GTC). namely (-) epicatechin (EC), (-) epicatechin gallate (ECG), (-) epigallocatechin (EGC), and (-) epigallocatechin gallate (EGCG), have been studied extensively for their wide-ranging biological activities. The goal of the present study was to examine the stability of GTC as a mixture under various processing conditions. The stability study demonstrated that GTC was stable in water at room temperature. When it was brewed at 98 degrees C for 7 h, longjing GTC degraded by 20%. When longjing GTC and pure EGCG were autoclaved at 120 degrees C for 20 min, the epimerization of EGCG to (-) gallocatechin gallate (GCG) was observed. The relatively high amount of GCG found in some tea drinks was most likely the epimerization product of EGCG during autoclaving. If other ingredients were absent, the GTC in aqueous solutions was pH-sensitive: the lower the pH, the more stable the GTC during storage. When it was added into commercially available soft drinks or sucrose solutions containing citric acid and ascorbic acid, longjing GTC exhibited varying stability irrespective of low pH value. This suggested that other ingredients used in production of tea drinks might interact with GTC and affect its stability. When canned and bottled tea drinks are produced, stored, and transported, the degradation of GTC must be taken into consideration.     

The stability of soft drinks intake from adolescence to adult age and the association between long-term consumption of soft drinks and lifestyle factors and body weight

OBJECTIVES: To investigate the tracking of sugar-sweetened, carbonated soft drinks intake from age 15 to 33 years and the association between this intake and lifestyle factors and body weight. DESIGN: A longitudinal study with 18-20 years of follow-up. Data about diet, physical activity, smoking and dieting were collected in 1981/1979, 1991 and 1999. Body weight and height were measured in 1981/1979 and self-reported in 1999. SETTING: Oslo, Norway. SUBJECTS: Four hundred and twenty-two men and women. RESULTS: Tracking of soft drinks intake from adolescence into early adulthood (age 25 years) and from early adulthood into later adulthood (33 years) was moderate to high, while tracking from adolescence into later adulthood was low. Comparing those reporting a high intake of soft drinks in both 1991 and 1999 with those reporting a low intake at both times, male long-term high consumers were more likely to smoke (48 vs. 21%, P=0.002) and reported higher intakes of energy (12.2 vs. 10.2 MJ day(-1), P=0.005) and sugar (142 vs. 50 g day(-1), P<0.001) in 1999 than did long-term low consumers. Women high consumers were less likely to be physically active (14 vs. 42%, P=0.03) and had higher sugar intake (87 vs. 41 g day(-1), P<0.001) in 1999 than did women low consumers. There were no differences in body mass index, overweight or obesity in 1999 between long-term high and low consumers. CONCLUSION: In this study, stability of soft drinks intake from age 15 to 25 years and from age 25 to 33 years was moderate to high, while from age 15 to 33 years it was low. Soft drinks intake from age 25 to 33 years was associated with smoking and physical inactivity, but not with body weight.     

Discrimination and classification of olive tree varieties and cultivation zones by biophenol contents

The peak areas from a high-performance liquid chromatography-diode array (HPLC-DAD) analysis of biophenols extracted from olive leaves have been used as chemotaxonomic markers to construct chemometric models in order to discriminate and classify (1) 13 varieties of Olea europaea olive trees, namely, Alame?o, Arbequina, Azulillo, Chorna, Hojiblanca, Lechín, Manzanillo, Negrillo, Nevadillo, Ocal, Pierra, Sevillano, and Tempranillo, from the same cultivation zone and (2) Arbequina samples from six different geoghaphical origins, namely, Córdoba, Mallorca (north and south), Ciudad Real, Lleida, and Navarra. Models based on principal component analysis (PCA) and hierarchical cluster analysis (HCA) were used for discrimination between samples as a function of the tree varieties and cultivation zone, whereas K nearest neighbors (KNN) and soft independent modeling of class analogy (SIMCA) models were generated to classify the samples used to validate the models into one of the groups previously established by PCA and HCA. KNN classified correctly 93 and 92% of the samples into the variety and cultivation zone, respectively; meanwhile, the SIMCA models predicted 85 and 92%, respectively.