Gas chromatographic determination of isocitric and malic acid in the presence of a large excess of citric acid

Derivatization yields of different esters (methyl, ethyl, n-propyl, isopropyl, n-butyl and isobutyl) of citric, malic and isocitric acids with various acylating agents, such as acetic anhydride, propionic anhydride, trifluoroacetic anhydride and heptafluorobutyric anhydride, were investigated. The formation of acylated malic and isocitric acid esters is rapid and quantitative whereas the acylation of citric acid esters was slow and partial in most instances. It was found that selective analytical conditions can be achieved with the O-heptafluorobutyryl n-butyl esters. The analytical applicability of the separation and determination of the malic, isocitric and citric acid contents of model solutions and of pressed lemon juice is discussed. Concentrations of 1.2 × 10^?3 ?9.0 × 10^?3g per 100 g of isocitric acid and 4.2 × 10^?3 ?3.5 × 10^?2 g per 100 g of malic acid in the presence of 9.3 × 10^?1 g per 100 g of citric acid were measured with relative standard deviations of 7.5 and 4.2%, respectively.     

Determination of α‐hydroxy acids and their enantiomers in fruit juices by ligand exchange CE with a dual central metal ion system

The content of α‐hydroxy acids and their enantiomers can be used to distinguish authentic and adulterated fruit juices. Here, we investigated the use of ligand exchange CE with two kinds of central metal ion in a BGE for the simultaneous determination of enantiomers of dl ‐malic, dl ‐tartaric and dl ‐isocitric acids, and citric acid. Ligand exchange CE with 100 mM d ‐quinic acid as a chiral selector ligand and 10 mM Cu(II) ion as a central metal ion could enantioseparate dl ‐tartaric acid but not dl ‐malic acid or dl ‐isocitric acid. Addition of 1.8 mM Sc(III) ion to the BGE with 10 mM Cu(II) ion to create a dual central metal ion system permitted the simultaneous determination of these α‐hydroxy acid enantiomers and citric acid. The proposed ligand exchange CE was thus well suited for detecting adulteration of fruit juices.     

Enzyme-assisted extraction and ionic liquid-based dispersive liquid–liquid microextraction followed by high-performance liquid chromatography for determination of patulin in apple juice and method optimization using central composite design

A simple and highly sensitive analytical methodology for isolation and determination of patulin in apple-juice samples, based on enzyme-assisted extraction (EAE) and ionic liquid-based dispersive liquid–liquid microextraction (IL-DLLME) was developed and optimized. Enzymes play essential roles in eliminating interference and increasing the extraction efficiency of patulin. Apple-juice samples were treated with pectinase and amylase. A mixture of 80 μL ionic liquid and 600 μL methanol (disperser solvent) was used for the IL-DLLME process. The sedimented phase was analyzed by high-performance liquid chromatography (HPLC). Experimental parameters controlling the performance of DLLME, were optimized using response surface methodology (RSM) based on central composite design (CCD). Under optimum conditions, the calibration curves showed high levels of linearity (R² > 0.99) for patulin in the range of 1–200 ng g⁻¹. The relative standard deviation (RSD) for the seven analyses was 7.5%. The limits of detection (LOD) and limits of quantification (LOQ) were 0.15 ng g⁻¹ and 0.5 ng g⁻¹, respectively. The merit figures, compared with other methods, showed that new proposed method is an accurate, precise and reliable sample-pretreatment method that substantially reduces sample matrix interference and gives very good enrichment factors and detection limits for investigation trace amount of patulin in apple-juice samples.     

Proton high‐field NMR study of tomato juice

A detailed analysis of the proton high‐field (600 MHz) NMR spectra of tomato juice and pulp is reported for the first time. A combination of J‐resolved, COSY, TOCSY, DOSY, ¹H–¹³C HSQC and ¹H–¹³C HMBC 2D sequences was used to assign each spin system and to separate the components of the complex patterns in the 1D overlapped proton spectra. To obtain resolved proton spectra of tomato pulps the high‐resolution magic angle spinning technique was used; a comparison with the liquid‐state NMR spectra of the corresponding juices was accomplished. On the basis of the assignments made, the chemical composition of tomato juices from two cultivars (Red Setter and Ciliegino) was determined. Copyright © 2003 John Wiley & Sons, Ltd.     

芜菁拮抗交通性污染物致小鼠遗传毒性效应的初步研究

以清洁级ICR小白鼠为实验动物,选择温州市鹿城区十里亭、火车站、南站交通岗亭为处理现场,采用小鼠骨髓嗜多染红细胞(PCE)的微核试验、小鼠精子畸形试验以及分光光度法测定小鼠肝脏过氧化氢酶(CAT)活性等实验方法,研究温州市区交通污染物对小鼠的遗传毒性及芜菁块根汁对它的拮抗效应.结果表明:经交通污染物处理的小鼠,其PCE的微核率、精子畸形率以及肝脏过氧化氢酶活性均明显高于阴性对照组;灌芜菁块根汁均可使小鼠PCE微核率、精子畸形率以及CAT活性明显下降,微核抑制率分别为62.96%、80.18%、87.36%,精子畸形抑制率分别为21.88%、45.89%、40.65%,CAT活性抑制率分别为17.27%、31.36%、37.76%.结论是交通性污染物对小鼠具有明显的遗传毒性效应;芜菁块根汁对交通性污染物引起小鼠遗传毒性效应具有显著的拮抗效应.     

Bioaccessibility of selected trace metals in urban PM<Subscript>2.5</Subscript> and PM<Subscript>10</Subscript> samples: a model study

Bioaccessibility of trace metals originating from urban particulate matter was assessed in a worst case scenario to evaluate the uptake and thus the hazardous potential of these metals via gastric juice. Sampling was performed over a period of about two months at the Getreidemarkt in downtown Vienna. Concentrations of the assayed trace metals (Ti, Cr, Mn, Co, Ni, Cu, Zn, Mo, Ag, Cd, Sn, Sb, Tl and Pb) were determined in PM_2.5 and PM₁₀ samples by ICP-MS. The metal concentrations in sampled air were in the low picogram to high nanogram per cubic metre range. The concentrations in PM_2.5 samples were generally lower than those in PM₁₀ samples. The average daily intake of these metals by inhalation for a healthy adult was estimated to be in the range of <1 ng (Tl) to >1,000 ng (Zn). To estimate the accessibility of the inhaled and subsequently ingested metals (i.e. after lung clearance had taken place) in the size range from 2.5- to 10-μm aerodynamic equivalent diameter, a batch-extraction with synthetic gastric juice was performed. The data were used to calculate the bioaccessibility of the investigated trace metals. Extractable fractions ranged from 2.10% (Ti in PM_2.5) to 91.0% (Cd in PM_2.5), thus yielding bioaccessible fractions (PM_2.5–10) from 0.16 ng (Ag) to 178 ng (Cu).     

Lycium Barbarum Polysaccharides and Wolfberry Juice Prevent DEHP-Induced Hepatotoxicity via PXR-Regulated Detoxification Pathway

Environmental di(2-Ethylhexyl) phthalate (DEHP) is widely used in various industries as a plasticizer, and has been reported to induce reproductive and developmental toxicities in organisms. The purpose of this study was to evaluate the detoxification capacity of Lycium barbarum polysaccharides (LBP) and wolfberry juice (WJ) against DEHP-induced hepatotoxicity. Two groups of rats were purchased to study two different intervention method experiments: LBP (50, 100, 200 mg/kg·bw) intervention before DEHP (2000 mg/kg·bw) exposure, and LBP (200 mg/kg·bw) or WJ (8 mL/kg·bw) intervention after DEHP (3000 mg/kg·bw) exposure. The rats were exposed to DEHP once, while the intervention lasted for seven days. At the end of the intervention, enzyme-linked immunosorbent assay (ELISA) was used to measure the related index. The LBP intervention before DEHP exposure experiment (the first experimental method) found that LBP group rats showed a strong capacity toward DEHP detoxification, evidenced by the significant upregulation of activities and concentrations of the partner retinoid, X receptor alpha (RXRα), and downstream regulators Cytochrome P4502E1 (CYP2E1), Cytochrome P4503A1 (CYP3A1), Glutathione S-Transferase Pi (GSTpi), and UDP-glucuronosyltransferase 1 (UGT1) in a dose-dependent manner. The LBP and WJ intervention after DEHP exposure experiment (the second intervention experiment) found that WJ could downregulate pregnane X receptor (PXR), and upregulate downstream regulators, CYP2E1, CYP3A1, and Glutathione S-Transferase (GST) with the extension of intervention time, to alleviate the toxicity of DEHP. However, the intervention effect of WJ was more obvious than that of LBP. These results suggested that LBP and WJ might be effective detoxification agents against DEHP-induced toxic effects, by activating PXR and PXR-related detoxifying enzymes.     

Impact of High-Pressure Homogenization Parameters on Physicochemical Characteristics,Bioactive Compounds Content,and Antioxidant Capacity of Blackcurrant Juice

High-pressure homogenization (HPH) is one of the food-processing methods being tested for use in food preservation as an alternative to pasteurization. The effects of the HPH process on food can vary depending on the process parameters used and product characteristics. The study aimed to investigate the effect of pressure, the number of passes, and the inlet temperature of HPH processing on the quality of cloudy blackcurrant juice as an example of food rich in bioactive compounds. For this purpose, the HPH treatment (pressure of 50, 150, and 220 MPa; one, three, and five passes; inlet temperature at 4 and 20 °C) and the pasteurization of the juice were performed. Titratable acidity, pH, turbidity, anthocyanin, vitamin C, and total phenolics content, as well as colour, and antioxidant activity were measured. Heat treatment significantly decreased the quality of the juice. For processing of the juice, the best were the combinations of the following: one pass, the inlet temperature of 4 °C, any of the used pressures (50, 150, and 220 MPa); and one pass, the inlet temperature of 20 °C, and the pressure of 150 MPa. Vitamin C and anthocyanin degradation have been reported during the HPH. The multiple passes of the juice through the machine were only beneficial in increasing the antioxidant capacity but negatively affected the colour stability.     

A White Grape Juice Extract Reduces Fat Accumulation through the Modulation of Ghrelin and Leptin Expression in an In Vivo Model of Overfed Zebrafish

A caloric surplus and a sedentary lifestyle are undoubtedly known to be the leading causes of obesity. Natural products represent valuable allies to face this problematic issue. This study was planned to assess the effect of a white grape (Vitis vinifera) juice extract (WGJe) in diet-induced obese zebrafish (Danio rerio). Fish were divided into four different diet groups: (i) normally fed (NF); (ii) overfed (OF); (iii) WGJe-supplemented NF (5 mL/L in fish water); (iv) WGJe-supplemented OF. Body mass index (BMI) was extrapolated each week. After the fourth week, euthanized zebrafish were processed for both microscopic evaluations and gene expression analyses. OF zebrafish showed higher BMI values with respect to NF counterparts, an effect that was hindered by WGJe treatment. Moreover, histological analyses showed that the area of the adipose tissue, as well as the number, size, and density of adipocytes was significantly higher in OF fish. On the other hand, WGJe was able to avoid these outcomes both at the subcutaneous and visceral levels, albeit to different extents. At the gene level, WGJe restored the altered levels of ghrelin and leptin of OF fish both in gut and brain. Overall, our results support the anti-obesity property of WGJe, suggesting its potential role in weight management.     

Application of ultrasonication at different microbial growth stages during apple juice fermentation by Lactobacillus plantarum: Investigation on the metabolic response

In this work, low-intensity ultrasonication (58.3 and 93.6 W/L) was performed at lag, logarithmic and stationary growth phases of Lactobacillus plantarum in apple juice fermentation, separately. Microbial responses to sonication, including microbial growth, profiles of organic acids profile, amino acids, phenolics, and antioxidant capacity, were examined. The results revealed that obvious responses were made by Lactobacillus plantarum to ultrasonication at lag and logarithmic phases, whereas sonication at stationary phase had a negligible impact. Sonication at lag and logarithmic phases promoted microbial growth and intensified biotransformation of malic acid to lactic acid. For example, after sonication at lag phase for 0.5 h, microbial count and lactic acid content in the ultrasound-treated samples at 58.3 W/L reached 7.91 ± 0.01 Log CFU/mL and 133.70 ± 7.39 mg/L, which were significantly higher than that in the non-sonicated samples. However, the ultrasonic effect on microbial growth and metabolism of organic acids attenuated with fermentation. Moreover, ultrasonication at lag and logarithmic phases had complex influences on the metabolism of apple phenolics such as chlorogenic acid, caffeic acid, procyanidin B2, catechin and gallic acid. Ultrasound could positively affect the hydrolysis of chlorogenic acid to caffeic acid, the transformation of procyanidin B2 and decarboxylation of gallic acid. The metabolism of organic acids and free amino acids in the sonicated samples was statistically correlated with phenolic metabolism, implying that ultrasound may benefit phenolic derivation by improving the microbial metabolism of organic acids and amino acids.