Determination of Gibberellin A3 residue in fruit samples by liquid chromatography–tandem mass spectrometry

A fast, simple, low cost, and high throughput method has been developed for the determination of Gibberellin A3 residue in fruit samples (apple, orange, peach, pear and grape). Analysis is performed by LC–MS/MS operated in the multiple reaction monitoring (MRM) mode, acquiring two specific precursor-product ion transitions per target compound. The method has been validated showing good linearity and selectivity. Limits of quantification (LOQs) were 10 μg kg⁻¹ for apple, orange, peach, pear and grape samples. The average recoveries, measured at three concentration levels (10, 20 and 200 μg kg⁻¹) were in the range 77.8–96.2% for the compound tested with relative standard deviations below 13.7%. The proposed method is rapid, simple and could be utilised for the routine analysis of Gibberellin A3 in fruit samples.     

Odor and taste thresholds of potential carry-over/off-flavor compounds in orange and apple juice

The odor and taste threshold values of six aroma substances known to be constituents of fruit juices and other fruit products, i.e. limonene, α-terpineol, carvone, methyl 2-methylbutanoate, ethyl 2-methylbutanoate, and γ-decalactone, were determined in various matrices, i.e. model sugar/acid solution, apple and orange juice, as well as apple and orange substitute (made by dilution of fruit juice concentrate with water). Whereas for α-terpineol thresholds in the 1.2-11 mg/l area were defined, limonene and carvone were determined to be sensorially effective each at 0.5 mg/l. Very low thresholds were measured for γ-decalactone, methyl 2-methylbutanoate and ethyl 2-methylbutanoate that showed sensory activity in the area of 20, 1.5, and 0.5 μg/l, respectively. In relation to the aroma composition determined by high resolution gas chromatography-mass spectrometry (HRGC-MS), these results provide an objective possibility to evaluate the sensory efficacy and/or an ‘off-flavor’ potential of these compounds in fruit juices.     

Brix degree and sorbitol/xylitol level of authentic pomegranate (Punica granatum) juice

With regard to 45 pomegranate fruits from different regions and several domestic varieties, fruit weight was found to be 137.1–738.2 g, peel share 34.4–73.1%, aril share 26.9–65.6% and fruit juice yield 19.2–48.0%. Brix degree of pomegranate juice samples obtained from the aforementioned fruits changed from 12.2 to 17.8 and was lower than 14.0 in approximately 18% of the samples. Titratable acidity of pomegranate juice samples varied between 2.4 and 30 g/L and the formol number varied between 4.0 and 20.0. The sorbitol/xylitol content ranged between 16 and 423 mg/L, mostly lying between 51 and 200 mg/L with a frequency of 64%. The share of samples containing sorbitol/xylitol higher than 250 g/L is 7%.     

Effect of enterocin AS-48 in combination with high-intensity pulsed-electric field treatment against the spoilage bacterium Lactobacillus diolivorans in apple juice

Enterocin AS-48 was tested in apple juice against the cider-spoilage, exopolysaccharide-producing strain Lactobacillus diolivorans 29 in combination with high-intensity pulsed-electric field (HIPEF) treatment (35 kV/cm, 150 Hz, 4 μs and bipolar mode). A response surface methodology was applied to study the bactericidal effects of the combined treatment, with AS-48 concentration and HIPEF treatment time as process variables. At subinhibitory bacteriocin concentrations, microbial inactivation by the combined treatment increased as the bacteriocin concentration and the HIPEF treatment time increased (from 0.5 to 2.0 μg/ml and from 100 to 1000 μs, respectively). Highest inactivation (4.87 logs) was achieved by 1000 μs HIPEF treatment in combination with 2.0 μg/ml AS-48. While application of treatments separately did not protect juice from survivors during storage, survivors to the combined treatment were inactivated within the following 24 h of storage, and the treated samples remained free from detectable lactobacilli for at least 15 days at temperatures of 4 °C as well as 22 °C. The combined treatment could be useful for inactivation of exopolysaccharide-producing L. diolivorans in apple juice.     

Occurrence of patulin and its dietary intake through apple juice consumption by the Spanish population

A survey was conducted to determine levels and dietary intake of Patulin (PAT) from apple juices consumed in Spain. One hundred samples of apple juice were bought from distinct supermarkets. PAT was extracted by a liquid–liquid extraction technique and analysed with a micellar electrokinetic chromatography (MEKC) method. 66% of the samples contained PAT over the limit of detection of the method (0.7 μg L⁻¹). The PAT apple juice mean and median levels obtained were 19.4 and 4.8 μg L⁻¹, respectively, in a range between 0.7 and 118.7 μg L⁻¹. In 11% of the samples, PAT contamination exceeded the maximum permitted level of 50 μg L⁻¹ established by the EU regulation. In Spain, no significant variations were observed with respect to data published 15 years ago.     

Determination of fenhexamid residues in grape must,kiwifruit, and strawberry samples by enzyme-linked immunosorbent assay

Fenhexamid is a new-generation agrochemical extensively used nowadays to protect high valuable crops and fruits from fungus attacks. In this paper, the development of an indirect competitive immunoassay for the determination of fenhexamid residues in fruit samples is described. After optimisation of immunoreagent concentrations, the assay, based on monoclonal antibody FHo4#27, showed high sensitivity, and selectivity, with a limit of detection for fenhexamid standards in buffer of 0.04 μg/L. The influence of several physico-chemical factors, including pH, ionic strength, solvent tolerance, and matrix interferences on the analytical parameters of the standard curve was studied. For spiked liquid food samples like grape must, just a direct 1:50 dilution in water was sufficient to attain recoveries between 100% and 110%. For kiwifruit and strawberry samples, a double extraction procedure with methanol is proposed in this study, which afforded recovery values that ranged between 103% and 116%. The limit of quantification of the developed assay was 5 μg/kg for grape must, 10 μg/kg for kiwifruits, and 25 μg/kg for strawberries. The optimised assay was compared with a reference procedure based on liquid chromatography using incurred samples from the market, and an excellent correlation between both methods was found.     

Application of a multi-pass high-pressure homogenization treatment for the pasteurization of fruit juices

This work evaluates both the effects of a multiple-pass high-pressure homogenization treatment on the microbial inactivation of selected microbial strains (Saccharomyces cerevisiae, Lactobacillus delbrueckii, Escherichia coli) inoculated into commercial fruit juices (orange, red orange, pineapple) as well as the application of this non-thermal technology to the pasteurization of fresh juices (Annurca apple juice). The pressure level ranged from 50 to 250 MPa, the number of passes from 1 to 5 and the inlet temperature from 2 to 20 °C.Preliminary tests in distilled water showed that the efficiency of the multiple-pass treatment significantly depends on both the homogenizing pressure as well as the microbial species. The subsequent extension of the multiple-pass treatment to the inactivation of S. cerevisiae inoculated into three different fruit juices (orange, red-orange and pineapple juice) highlighted that the inactivation induced by the high pressure treatment did not depend on the properties of the tested juices and was not statistically different from inactivation in water (p value < 0.05). These findings were supported by the comparison of two different mathematical models used to fit the inactivation kinetics, whose fitting parameters were not significantly different for water and the fruit juices for any pressure level applied.Three homogenization passes at 150 MPa and 25 °C, which resulted to be optimal for yeast inactivation in fruit juices, were effective for the stabilization of the endogenous microbial load of fresh Annurca apple juice. The treated apple juice showed a minimum shelf-life of 28 days under refrigerated conditions, during which the natural qualities of the fresh juice were completely preserved.     

Moulds and yeasts in fruit salads and fruit juices

Thirty-eight fruit salad samples including cantaloupe, citrus fruits, honeydew, pineapple, cut strawberries and mixed fruit salads, and 65 pasteurized fruit juice samples (apple, carrot, grapefruit, grape and orange juices, apple cider, and soy milk) were purchased from local supermarkets in the Washington, DC area and tested for fungal contamination. The majority of fruit salad samples (97%) were contaminated with yeasts at levels ranging from <2.0 to 9.72 log10 of colony forming units per gram (cfu/g). Frequently encountered yeasts were Pichia spp., Candida pulcherrima, C. lambica, C. sake, Rhodotorula spp., and Debaryomyces polymorphus. Low numbers of Penicillium spp. were found in pineapple salads, whereas Cladosporium spp. were present in mixed fruit and cut strawberry salads. Twenty-two per cent of the fruit juice samples tested showed fungal contamination. Yeasts were the predominant contaminants ranging from <1.0 to 6.83 log10 cfu/ml. Yeasts commonly found in fruit juices were C. lambica, C. sake, and Rhodotorula rubra. Geotrichum spp. and low numbers of Penicillium and Fusarium spp. (1.70 and 1.60 log10 cfu/ml, respectively) were present in grapefruit juice.     

Stability of black carrot anthocyanins in various fruit juices and nectars

Fruit juices (apple, grape, orange, grapefruit, tangerine and lemon) and nectars (apricot, peach and pineapple) were coloured with black carrot juice concentrate and stability of black carrot anthocyanins in these matrices was studied during heating at 70–90 °C and storage at 4–37 °C. Anthocyanin degradation, in all coloured juices and nectars, followed first-order reaction kinetics. During heating, black carrot anthocyanins in apple and grape juices showed higher stability than those in citrus juices at 70 and 80 °C. High stability was also obtained for the anthocyanins in peach and apricot nectars at these temperatures. Black carrot anthocyanins were the least stable in orange juice during both heating and storage. During storage, degradation of anthocyanins was very fast at 37 °C, especially in pineapple nectar. Refrigerated storage (4 °C) markedly increased the stability in all samples. Activation energies for the degradation of black carrot anthocyanins in coloured juices and nectars ranged from 42.1 to 75.8 kJ mol⁻¹ at 70–90 °C and 65.9–94.7 kJ mol⁻¹ at 4–37 °C.     

混合果汁起泡酒酿造工艺的研究

以苹果汁、葡萄汁、哈密瓜汁作为原料,对酿造复合型起泡酒的工艺进行研究。采用正规的“留糖法”进行发酵生产,酒中的CO2、酒精、酸糖皆来自于果汁。通过单因素及正交试验确定了葡萄苹果起泡酒最佳工艺条件为德国酵母3#,接种量0.8 g/L,葡萄汁与苹果汁质量比3∶2,发酵醪糖度16%,采用罐内发酵方式对起泡酒进行充气,CO2含量0.15 MPa。哈密瓜苹果起泡酒最佳工艺条件为德国酵母3#,接种量0.8 g/L,哈密瓜汁与苹果汁质量比1∶1,发酵醪糖度14%,采用罐内发酵方式对起泡酒进行充气,CO2含量0.13 MPa。由此最佳工艺条件得到的葡萄苹果起泡酒和哈密瓜苹果起泡酒,酒香和果香协调浓郁,口感酸甜均衡,酒体丰满,杀口力强,后味爽。     

Survey of South African fruit juices using a fast screening HILIC-MS method

Adulteration of fruit juices – by the addition of sugar or other less expensive fruit juices as well as preservatives, artificial sweeteners and colours – was tested for by using a developed screening method. The method employs hydrophilic interaction liquid chromatography-mass spectrometry (HILIC-MS) using electrospray ionisation in the negative mode and ultraviolet light detection. Different fruit juices can be differentiated by the content of marker compounds like sorbitol, certain phenolic molecules and their saccharide profile. This method was used to test 46 fruit juice samples from the retail market as well as 12 control samples. The study focused on the main types of fruit juices consumed on the South African market including apple, orange, grape and blends of these juices with other fruits like mango, pear and guava. Overall, the 46 samples tested mostly agreed with label claims. One grape juice sample was adulterated, probably with apple juice. Natamycin above the legal limits was found in two samples. In addition, two samples contained natamycin and one sample benzoate without it being indicated on the label. The method is well suited as a quick screening method for fruit juice adulteration and if used routinely would reduce fruit juice adulteration without the cost of the current array of tests needed for authenticity testing.     

Impact of apple processing modes on extracted juice quality: Pressing assisted by pulsed electric fields

The purpose of this study was to compare the effects of pulsed electric field (PEF) on apple juice characteristics (turbidity, polyphenolic content and antioxidant capacities). The pressing was used as a standard method for juice extraction. Experiments were carried out at a constant pressure (P = 3 bar) using a laboratory press cell. Two different methods for PEF application at 400 V/cm were investigated (PEF treatment of whole samples before cutting and PEF treatment of apple slices after cutting). PEF treatment resulted in increase of the juice yield from 44 g/100 g apple (untreated samples) to 58 g/100 g apple (treatment of whole apples) and 64 g/100 g apple (treatment of slices) after 30 min of pressing. The analysis of pH and conductivity showed no significant difference between untreated and PEF-treated samples. However, the total soluble matter content of juice increased after PEF treatment. The obtained turbidity and transmittance data evidence a noticeable improvement of juice clarity for PEF-treated samples. The PEF pre-treatment was accompanied by an increase of the content of polyphenols and intensification of the antioxidant capacities of juice. Most of these effects (juice clarity and content of antioxidants) were more pronounced for the whole treated apples as compared to untreated apples and PEF-treated apple slices. The evolution of apple browning before and after PEF treatment was more pronounced for whole samples. PEF treatment accelerates browning. The obtained data can contribute to the determination of an optimum time for PEF application. The results evidence that PEF-enhanced expression is promising for production of higher quality juices. PEF treatment of whole apples reduces the energy consumption and is advantageous for industrial applications as compared to the treatment of apple slices. PEF combined with pressing can become a good alternative to traditional process.     

Prebiotic effect of fermented cashew apple (Anacardium occidentale L) juice

Leuconostc mesenteroides B-512F and L. mesenteroides B-742 were cultivated in clarified cashew apple juice to produce prebiotic oligosaccharides. Yeast extract (20 g/L); K₂HPO₄ (g/L) and sucrose (50 g/L) were added to the juice to promote the microbial growth and dextransucrase production. Initial pH was adjusted to 6.5 with H₃PO₄. Fermentations were carried out at 30 °C and 150 rpm for 24 h. The prebiotic effect of the fermented cashew apple juice, containing oligosaccharides, was evaluated through the Lactobacillus johnsonii B-2178 growth. L. johnsonii was incubated for 48 h using fermented cashew apple juice as substrate. Lactobacillus growth was compared to the microbial growth in non-fermented juice and in MRS broth. L. johnsonii growth in the fermented cashew apple juice was threefolds the observed growth in the non-fermented juice.     

Simultaneous estimation of the thermophysical properties of three kinds of fruit juices based on the measured result by a transient heat flow probe method

The thermophysical properties of three kinds of fruit juices (grape juice, orange juice, and pineapple juice) were measured at various temperatures (10–50 °C) and concentrations (10–50%). A new method for the simultaneous determination of thermophysical properties using a modified version of current probe theory method was proposed. The temperature changes of the probe upon insertion in the sample were fitted to an approximate solution of the heat conduction equation, and the values of two parameters in that solution were determined. Using the values of these parameters, the thermal conductivity and thermal diffusivity of each sample were determined. The specific heat of each sample was estimated from the definition of thermal diffusivity. These thermophysical properties were expressed as a function of concentration and temperature.     

Processing and analytical characterisation of pulp-enriched cloudy apple juices

Pulp-enriched cloudy apple juices were manufactured from two apple varieties by blending of apple puree with natural cloudy apple juice in order to enrich bioactive secondary plant substances. Finishing of the puree with a 0.6-mm mesh screen and final product homogenisation revealed as the optimum processing technology for the novel 100% fruit beverage. The presence of large particles originating from the puree prevented long-term cloud stability, but due to the proportion of cloud-stable juice a complete phase separation did not occur. Optimal drinkability was achieved at a viscosity of 11.5 mPa s. Polyphenol compositions and concentrations were determined by means of RP-HPLC/PDA. The results ranged from 109 to 610 mg/l. All samples showed the typical polyphenol pattern of apples with dominating hydroxycinnamic acids followed by flavanols and flavonols. The puree addition to the cloudy apple juices increased the polyphenol concentrations by average 100%. Relatively, the highest increase could be observed for dimeric procyanidins. Different technological variants did not affect significantly the polyphenol concentrations. The dietary fibre contents of the pulp-enriched cloudy apple juices ranged from 5.8 to 9.4 g/l.     

Comparison of Simple and Rapid Extraction Procedures for the Determination of Pesticide Residues in Fruit Juices by Fast Gas Chromatography–Mass Spectrometry

Three sample treatment methods, based on QuEChERS, solid-phase extraction (SPE) and solid-phase microextraction (SPME), were compared and evaluated in order to obtain the best conditions to determine pesticide residues in fruit juice by fast gas chromatography–mass spectrometry (single quadrupole GC-MS). Analysis were performed under selected ion monitoring, acquiring the three most abundant and/or specific ions for each analyte and using their relative intensity ratios as a confirmatory parameter. The 3 methodologies (QuEChERS, SPE and SPME) were validated taking 15 selected pesticides as model compounds, using commercial apple juice. QuEChERS procedure was based on the AOAC Official Method 2007.01, using acetonitrile (containing 1 % acetic acid) as extraction solvent and primary–secondary amine during the dispersive solid-phase extraction. Oasis hydrophilic–lipophilic balance cartridges were used for SPE, and polyacrylate fibers were used for direct immersion SPME procedure. Three isotopically labeled standards were added to the samples before extraction and used as surrogate standards. Validation parameters as recoveries, limits of detection, and limits of quantification (LOQ), as well as matrix effects and sample throughput, were obtained and compared for the three extraction procedures. QuEChERS was considered faster and led to the best quantitative results. In this way, validation was extended to up to 56 pesticides by applying QuEChERS in multi-fruit juice samples, obtaining LOQs ranging from 2 to 20 μg/L for most compounds. Accuracy and precision were evaluated by means of recovery experiments at two concentration levels (10 and 100 μg/L), obtaining recoveries between 70 and 120 % in most cases and relative standard deviations below 15 %. Finally, the QuEChERS method was applied to the analysis of commercial juices, including mango–apple, pineapple, grapefruit and orange.     

The use of photochemiluminescence for the measurement of the integral antioxidant capacity of baobab products

The number of methods to measure antioxidants in botanicals, foods, nutraceuticals and other dietary supplements are increased considerably in the last 10 years. However most techniques require long experimental times and high costs to determine antioxidant capacity of hydrophilic or lipophilic compound in a food mixture. By means of a photochemiluminescence method, we assessed the Integral Antioxidant Capacity (IAC) which represents the sum of the antioxidant capacity of hydrophilic and lipophilic antioxidants. In this study the IAC of extracts from Adansonia digitatata (i.e. red fiber, fruit pulp and leaves), was assessed in comparison to those deriving from other natural sources of antioxidants (i.e. orange, kiwi, apple and strawberry). When compared, IAC values for the examined product resulted as follows: Adansonia digitata red fibre ? Adansonia digitata fruit pulp ? Adansonia digitata fresh leaves ? Adansonia digitata seeds ? Adansonia digitata radix cuticle ? orange fresh pulp ? strawberry fresh fruit pulp > Adansonia digitata radix > bilberry fresh pulp ? kiwi fruit pulp. Results clearly indicate the interesting antioxidants properties of Adansonia digitata red fibre, in particular the IAC value of baobab red fibre was 66 time higher than that of orange pulp, with value of 1617.3 μmol/g and 24.3 μmol/g, respectively.     

Determination of patulin in apple and quince products by GC–MS using C5–7 patulin as internal standard

A reliable gas chromatographic mass spectrometric method has been validated for the determination of trace levels (<10 μgL⁻¹) of patulin in apple products and quince jam. The method was based on extraction of patulin with ethyl acetate-hexane, alkalinisation and silylation with N,O-bis-trimethylsilyltrifluoroacetamide with 1% of trimethylchloro-silane. The accurate determination of patulin was achieved by employing commercial ¹³C_5–7 patulin labelled as an internal standard, which allowed compensating target analyte losses and enhancement or suppression matrix effects. Limits of detection and quantification of method using real samples were 0.4 and 1.6 μgkg⁻¹, respectively. Recoveries of patulin from samples spiked at 8–50 μgkg⁻¹ levels ranged between 71% and 89%. The repeatability of measurements (expressed as relative standard deviation) was lower than 16%. The method was successfully applied to the determination of patulin in apple fruit and apple products including juice, cider and baby food, and also in quince fruit and quince jam. A new PCR system for the detection of Penicillium expansum in samples containing highly degraded DNA was developed which permitted the detection of the mould in 2/3 of the samples containing patulin, including juices and jams.     

GC–MS quantification and sensory thresholds of guaiacol in orange juice and its correlation with Alicyclobacillus spp.

Guaiacol is a profoundly negative taint/off-flavour produced by the increasingly common microbial contamination of fruit juices with Alicyclobacillus spp. The objectives of this study included: determining sensory thresholds for guaiacol in orange juice (OJ), developing an analytical method whose detection limits were equivalent to sensory thresholds and determining levels of Alicyclobacillus spp. that would produce detectable levels of guaiacol. A 12 member trained panel was used to establish guaiacol detection and recognition thresholds. Guaiacol ortho and retro nasal detection thresholds in OJ were 0.70 and 0.53 μg/l respectively. Odour recognition threshold was 2.0 μg/l. A SPME GC–MS Selected Ion Monitoring (SIM) procedure was optimised to achieve analytical detection limits of 0.5 μg/l. Optimum guaiacol detection limit was achieved using only responses from m/z 109 and 124. Ion ratios (m/z 109/124) and linear retention index value matching were used to confirm the identification of guaiacol. Quantification was achieved using peak areas from standard guaiacol additions in orange juice between 0.5 and 100 μg/l. Alicyclobacillus growth of 2.2 log CFU/ml in OJ produced just detectable levels (0.7 μg/l) of guaiacol.     

Occurrence of patulin in various fruit juices from South Korea: An exposure assessment

To determine patulin in various fruit juices, high performance liquid chromatography (HPLC) method was optimized and validated. For validation of HPLC method, a linearity, accuracy, precision, detection limit, and quantification limit were determined. Linearity (R² = 0.99995), accuracy (96.1–115.7%), precision (3.31–9.52), detection limit (6 ng/mL), and quantification limit (8 ng/mL) were in agreement with performance criteria for patulin as set by the European Commission hence proved that HPLC can be used to detect patulin in fruit juices. After validation, the method was applied to estimate the prevalence of patulin in fruit juices (apple, grape, and orange juices). Nine samples (12.5%, 3 apple, 2 orange, and 4 grape juices) of 72 samples were positive for patulin in the range 2.8 to 30.9 ng/mL. According to the monitoring results, daily intake was estimated to be 0.17 ng/kg BW/day which was lower than the provisional maximum tolerable daily intake (0.4 μg/kg) established by Joint Expert Committee on Food Additives. These results indicate that the detection method coincides with the performance criteria and is appropriate for analysis of patulin, and continuous monitoring of patulin in various fruit juices from Korea is necessary.