Graphene oxide as a micro‐solid‐phase extraction sorbent for the enrichment of parabens from water and vinegar samples

A simple hydrophilic polyamide organic membrane protected micro‐solid‐phase extraction method with graphene oxide as the sorbent was developed for the enrichment of some parabens from water and vinegar samples prior to gas chromatography with mass spectrometry detection. The main experimental parameters affecting the extraction efficiencies, such as the type and amount of the sorbent, extraction time, stirring rate, salt addition, sample solution pH and desorption conditions, were investigated. Under the optimized experimental conditions, the method showed a good linearity in the range of 0.1–100.0 ng/mL for water samples and 0.5–100.0 ng/mL for vinegar samples, with the correlation coefficients varying from 0.9978 to 0.9997. The limits of detection (S/N = 3) of the method were in the range of 0.005–0.010 ng/mL for water samples and 0.01–0.05 ng/mL for vinegar samples, respectively. The recoveries of the method for the analytes at spiking levels of 5.0 and 70.0 ng/mL were between 84.6 and 106.4% with the relative standard deviations varying from 4.2 to 9.5%. The results indicated that the developed method could be a practical approach for the determination of paraben residues in water and vinegar samples.     

Webcam camera as a detector for a simple lab-on-chip time based approach

A modification of a webcam camera for use as a small and low cost detector was demonstrated with a simple lab-on-chip reactor. Real time continuous monitoring of the reaction zone could be done. Acid-base neutralization with phenolphthalein indicator was used as a model reaction. The fading of pink color of the indicator when the acidic solution diffused into the basic solution zone was recorded as the change of red, blue and green colors (%RBG.) The change was related to acid concentration. A low cost portable semi-automation analysis system was achieved.     

Quantitative determination of polyalcohols in wine and vinegar by gas chromatography

Summary A gas chromatographic method is described for the analysis of arabitol, mannitol, sorbitol and inositol in wine. The method is evaluated for repeatability using perseitol as internal standard. Perseitol can be added to wine before or after passing the wine through the ion-exchange column without showing significant differences in the polyalcohol content. The method is also applied to the analysis of vinegar from different substrates (wine cider and rice).     

Multi-objective optimisation strategy based on desirability functions used for chromatographic separation and quantification of l-proline and organic acids in vinegar

An optimisation strategy based on desirability functions together with experimental design has been used to optimise a chromatographic method applied to the separation and quantification of l-proline and seven organic acids in vinegar samples. Chromatographic problems often force to reach a compromise between different experimental variables in order to achieve the best chromatographic separation. The importance of the use of multi-objective optimisation methods lies in the ability to cope with this kind of problems. The quality of the multicriteria optimisation method was tested through the validation of the analytical parameters of the final chromatographic method developed. The versatility of this methodology allows to use it in other chromatographic applications resulting in a suitable adaptive procedure to solve new analytical problems. Furthermore, the determination of l-proline and organic acids in vinegar is useful for several industrial goals such as the correct monitoring of fermentation, for the study of nutrient needs at all times during the twofold fermentation process and for the detection of possible adulterations in the final product.     

Comparative analysis of the organic acid content of vinegar by capillary electrophoresis and ion-exclusion chromatography with conductimetric detection

Summary Ion-exclusion chromatography (IEC) and capillary electrophoresis (CE) have been compared for determination of organic acids in samples of Sherry wine vinegar. The accuracy of each technique was evaluated by use of the standard addition method. There were no differences between the techniques at a significance level of 5%, except for determination of malic acid by CE. Both analytical methods were used to analyse sixteen samples of Sherry wine vinegar supplied by different producers. The regression coefficients (r ²) for analysis by IEC and CE exceeded 0.94 for all acids. Results from both methods were in good agreement and the methods are sufficiently selective and sensitive to be applied directly to sherry wine vinegars.     

Evaluation of Bi as internal standard to minimize matrix effects on the direct determination of Pb in vinegar by graphite furnace atomic absorption spectrometry using Ru permanent modifier with co-injection of Pd/Mg(NO3)2

Bismuth was evaluated as an internal standard for the direct determination of Pb in vinegar by graphite furnace atomic absorption spectrometry using Ru as a permanent modifier with co-injection of Pd/Mg(NO₃)₂. The correlation coefficient of the graph plotted from the normalized absorbance signals of Bi versus Pb was r = 0.989. Matrix effects were evaluated by analyzing the slope ratios between the analytical curve obtained from reference solutions prepared in 0.2% (v/v) HNO₃ and analytical curves obtained from Pb additions in red and white wine vinegar samples. The calculated ratios were around 1.04 and 1.02 for analytical curves established applying an internal standard and 1.3 and 1.5 for analytical curves without. Analytical curves in the 2.5–15 μg L^− 1 Pb concentration interval were established using the ratio Pb absorbance to Bi absorbance versus analyte concentration, and typical linear correlations of r = 0.999 were obtained. The proposed method was applied for direct determination of Pb in 18 commercial vinegar samples and the Pb concentration varied from 2.6 to 31 μg L^− 1. Results were in agreement at a 95% confidence level (paired t-test) with those obtained for digested samples. Recoveries of Pb added to vinegars varied from 96 to 108% with and from 72 to 86% without an internal standard. Two water standard reference materials diluted in vinegar sample were also analyzed and results were in agreement with certified values at a 95% confidence level. The characteristic mass was 40 pg Pb and the useful lifetime of the tube was around 1600 firings. The limit of detection was 0.3 μg L^− 1 and the relative standard deviation was ≤ 3.8% and ≤ 8.3% (n = 12) for a sample containing 10 μg L^− 1 Pb with and without internal standard, respectively.     

NMR relaxation data for quality characterization of Balsamic vinegar of Modena

In this paper, 22 samples consisting of Balsamic vinegar of Modena and two Traditional Balsamic vinegar of Modena samples have been analyzed by means of ¹H NMR spectroscopy. Some selected resonances have been used for quantification and for T1 (spin-lattice relaxation time) measurements. Statistical protocols applied to NMR data for quantification of selected resonances revealed the possibility to differentiate the samples according to their ageing process. Additionally, T1 measurements revealed a strong correlation with the ageing process and these new data were added for improving the statistical model, which was used to predict T1 relaxation time of selected compounds for Balsamic vinegar samples. Our results indicate that the use of NMR data and statistical methods is a valid approach that can be successfully used for ageing characterization of Balsamic vinegar of Modena samples.     

Establishing a sensitive capillary electrophoresis‐UV method for direct determination of amino acids to evaluate vinegar quality

In this study, the capillary electrophoresis method with ultraviolet detection was established to directly determine amino acids in vinegar, according to the coordination interaction between amino acids (AAs) and copper ions. The online sweeping technique was combined to improve the detection sensitivity. The quality of vinegar was evaluated with AAs as parameters by United Nations Food Agriculture Organization/Word Health Organization AAs model and principal component analysis. Optimum conditions were obtained under 50 mM CuSO₄ and adjusted pH 4.40 with 8 mM acetate, 70 s injection time, 22.5 kV separation voltage, and 254 nm detected wavelength. Method validation, indicating good linearity (R² > 0.9989), precision with an RSD less than 8.0% (n = 5), LOD (0.13–0.25 μg/mL), LOQ (0.43–0.83 μg/mL) and recovery (80.5–112.6%). Under the optimal conditions, AAs in vinegar can be directly separated which is propitious for the quality evaluation of vinegar.     

醋渍鸡蛋钙含量变化的研究

钙是人体必需元素之一，根据我国人民的膳食构成及营养状况，膳食中的钙摄入量尚不够充足，为寻找提高钙摄入量的途径，作者对醋渍鸡蛋，蛋壳和醋中的钙含量进行了测定。结果表明：醋渍８天的鸡蛋白每１００ｇ含钙量可达６００ｍｇ左右，相当于正常鸡蛋的１２倍，渍蛋和渍蛋壳（８％）３天后的醋，每１００ｍＬ含钙量约８００ｍｇ，相当于普通食醋的２１倍左右，因此，作者认为食用醋渍鸡蛋，醋渍蛋壳和渍蛋后的醋，均可提高国人膳食     

Liquid–liquid extraction of silylated polyalcohols from vinegar,and their determination by capillary GC

A capillary gas chromatographic method has been developed for the determination of glycerol, erythritol, arabitol, sorbitol, and inositol in vinegar. After addition of phenyl-β-glucopyranoside as internal standard, the sample was then dried and silylated. The analysis was performed both on the crude silylated sample and after liquid – liquid extraction. The repeatability of the two methods was evaluated on twenty three different types of vinegar and the extraction did not seriously affect the analysis. Extraction of the TMS-ethers enables elimination of a large number of interfering substances such as acids and polyphenols and so acts as a purification of the sample.