Effects of High-Pressure Treatment on the Sensory Quality of White Grape Juice

The effects of high-pressure treatment on the colour (objective measurement) and sensory characteristics of white grape juice were studied during storage at 4 °C for 60 days. Grape juice was subjected to three different treatments: 400 or 500 MPa at 2 u °C, and 400 MPa at 40 °C during 10 min. Untreated juice was used as control. Colour parameters (CIE L * a * b *), hue angle (tan m 1 b */ a *), chroma {( a * 2 + b * 2 ) 1/2 }, luminosity Q *{(10 2 log( L *) + 100} and saturation S *( C */ L *) were measured. Juices were evaluated for sweetness, acidity, off-flavour and aroma. High-pressure treatments did not affect the colour parameters of juice, and similar sensory characteristics were observed in both control and treated samples on the first day. The colour and sensory characteristics of pressure-treated samples remained more stable than those of the control juice during 60 days of storage. The control juice was slightly fermented developing some changes in flavour and colour.     

超声雾化顶空单滴微萃取-气相色谱-质谱法测定果汁中的芳香成分

本文建立了超声雾化顶空单滴微萃取-气相色谱-质谱(GC-MS)联用测定果汁中的β-月桂烯、D-柠檬烯和异戊酸叶醇酯含量的方法。考察了萃取溶剂、萃取时间、富集时间等影响芳香成分萃取效率的因素。在最优的实验条件下,对三种果汁中的芳香成分进行了分析,测得三种果汁中β-月桂烯、D-柠檬烯和异戊酸叶醇酯的含量分别为12.0~488.6μg·mL~(-1)、542.8~1.237×10~4μg·mL~(-1)和0.0470~498.5μg·mL~(-1)。方法的回收率范围为78.5%~110.4%,相对标准偏差为1.3%~4.4%。     

Magnetite Nanoparticles Immobilized Pectinase: Preparation,Characterization and Application for the Fruit Juices Clarification

In this work, pectinase was immobilized on the surface of silica‐coated magnetite nanoparticles via covalent attachment. The magnetite‐immobilized enzyme was characterized by Fourier transform infrared spectroscopy, X‐ray powder diffraction, scanning electron microscopy and vibrating sample magnetometery techniques. Response Surface Methodology using Minitab Software was applied for statistical designing of operating conditions in order to immobilize pectinase on magnetic nanoparticles. The optimal conditions were obtained at 30 °C and pH 5.5 with 42.97 μl pectinase for 2 h. The immobilization yield was 50.6% at optimized conditions. Compared to the free pectinase, the immobilized pectinase was found to exhibit enhanced enzyme activity, better tolerance to the variation of pH and temperature, and improved storage stability. Both free and immobilized samples reduced the viscosity of apple juice from 1.12 to 0.88 and 0.92 mm²s^?1, respectively, after 30 min at their optimum temperature. Furthermore, the immobilized enzyme could be reused six consecutive cycles and the efficiency loss in viscosity reduction was found to be only 8.16%.     

Effervescence‐assisted dispersive liquid–liquid microextraction using a solid effervescent agent as a novel dispersion technique for the analysis of fungicides in apple juice

A novel effervescence‐assisted dispersive liquid–liquid microextraction method has been developed for the determination of four fungicides in apple juice samples. In this method, a solid effervescent agent is added into samples to assist the dispersion of extraction solvent. The effervescent agent is environmentally friendly and only produces an increase in the ionic strength and a negligible variation in the pH value of the aqueous sample, which does not interfere with the extraction of the analytes. The parameters affecting the extraction efficiency were investigated including the composition of effervescent agent, effervescent agent amount, formulation of effervescent agent, adding mode of effervescent agent, type and volume of extraction solvent, and pH. Under optimized conditions, the method showed a good linearity within the range of 0.05–2 mg/L for pyrimethanil, fludioxonil, and cyprodinil, and 0.1–4 mg/L for kresoxim‐methyl, with the correlation coefficients >0.998. The limits of detection for the method ranged between 0.005 and 0.01 mg/L. The recoveries of the target fungicides in apple juice samples were in the range of 72.4–110.8% with the relative standard deviations ranging from 1.2 to 6.8%.     

On-capillary sample cleanup method for the electrophoretic determination of carbohydrates in juice samples

On many occasions, sample treatment is a critical step in electrophoretic analysis. As an alternative to batch procedures, in this work, a new strategy is presented with a view to develop an on-capillary sample cleanup method. This strategy is based on the partial filling of the capillary with carboxylated single-walled carbon nanotube (c-SWNT). The nanoparticles retain interferences from the matrix allowing the determination and quantification of carbohydrates (viz glucose, maltose and fructose). The precision of the method for the analysis of real samples ranged from 5.3 to 6.4%. The proposed method was compared with a method based on a batch filtration of the juice sample through diatomaceous earth and further electrophoretic determination. This method was also validated in this work. The RSD for this other method ranged from 5.1 to 6%. The results obtained by both methods were statistically comparable demonstrating the accuracy of the proposed methods and their effectiveness. Electrophoretic separation of carbohydrates was achieved using 200 mM borate solution as a buffer at pH 9.5 and applying 15 kV. During separation, the capillary temperature was kept constant at 40 degrees C. For the on-capillary cleanup method, a solution containing 50 mg/L of c-SWNTs prepared in 300 mM borate solution at pH 9.5 was introduced for 60 s into the capillary just before sample introduction. For the electrophoretic analysis of samples cleaned in batch with diatomaceous earth, it is also recommended to introduce into the capillary, just before the sample, a 300 mM borate solution as it enhances the sensitivity and electrophoretic resolution.     

Air-assisted liquid–liquid microextraction by solidifying the floating organic droplets for the rapid determination of seven fungicide residues in juice samples

A novel air assisted liquid–liquid microextraction using the solidification of a floating organic droplet method (AALLME-SFO) was developed for the rapid and simple determination of seven fungicide residues in juice samples, using the gas chromatography with electron capture detector (GC-ECD). This method combines the advantages of AALLME and dispersive liquid–liquid microextraction based on the solidification of floating organic droplets (DLLME-SFO) for the first time. In this method, a low-density solvent with a melting point near room temperature was used as the extraction solvent, and the emulsion was rapidly formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent for ten times repeatedly using a 10-mL glass syringe. After centrifugation, the extractant droplet could be easily collected from the top of the aqueous samples by solidifying it at a temperature lower than the melting point. Under the optimized conditions, good linearities with the correlation coefficients (γ) higher than 0.9959 were obtained and the limits of detection (LOD) varied between 0.02 and 0.25 μg L⁻¹. The proposed method was applied to determine the target fungicides in juice samples and acceptable recoveries ranged from 72.6% to 114.0% with the relative standard deviations (RSDs) of 2.3–13.0% were achieved. Compared with the conventional DLLME method, the newly proposed method will neither require a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly.     

Determination of limonoate and nomilinoate A-ring lactones in citrus juices by liquid chromatography-electrospray ionization mass spectrometry

The development of delayed bitterness in citrus products is a major problem to citrus producers and juice processors worldwide. A rapid and sensitive liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) method has been developed to quantify the recognized precursors of limonoid derived delayed bitterness, limonoate and nomilinoate A-ring lactones, in a wide variety of citrus juices. The limonoid A-ring lactones were isolated by solid-phase extraction from juice samples, analyzed by negative ion LC-ESI-MS and quantified utilizing the standard addition method.     

Multiresidue determination of pesticides in juice by solid-phase extraction and gas chromatography-mass spectrometry

A multiresidue method based on solid-phase extraction was developed for the simultaneous determination of 50 pesticides in commercial juices. The extraction procedure was carried out in C₁₈ columns preconditioned with acetonitrile and water. The subsequent elution of pesticides was performed with a mixture of hexane-ethyl acetate (1:1, v/v) prior to the determination by gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC-MS-SIM), using one target and two qualifier ions. Standards were prepared spiking blank juice samples to counteract the observed matrix effect. Average recoveries for all the pesticides studied were higher than 91% with relative standard deviations lower than 9% in the concentration range of 0.02-0.1 μg/mL and the detection limits achieved ranged from 0.1 to 4.6 μg/L. The proposed method was applied to the analysis of these compounds in commercial juices and diazinon, ethion and procymidone were the pesticides encountered, although the levels found were very low.     

Liquid–liquid microextraction methods based on ultrasound-assisted emulsification and single-drop coupled to gas chromatography–mass spectrometry for determining strobilurin and oxazole fungicides in juices and fruits

Two procedures are proposed based on ultrasound-assisted emulsification and single-drop liquid–liquid microextraction for the sensitive determination of seven strobilurin and six oxazole fungicides in fruits and juice samples. Both miniaturized techniques are coupled to gas chromatography with mass spectrometry in the selected ion monitoring mode, GC–MS(SIM). The procedures use low density organic solvents, and several factors influencing the emulsification, extraction and collection efficiency are optimized. The detection limits obtained at a signal-to-noise ratio of 3 are below the MRLs set by the European Commission. Enrichment factors are between 140–1140 for the first technique used and 80–1600 for the latter. The recoveries obtained for spiked samples are satisfactory for all compounds. The methods are validated according to the Commission Decision 2002/657/EC. Different fruit and juices are analyzed by the proposed method and none of the samples contained fungicide residues above the detection limits.     

液相微萃取-高效液相色谱法分析葡萄汁中多酚类化合物

建立了一种基于液相微萃取与高效液相色谱联用技术测定葡萄汁中鞣花酸、白藜芦醇和槲皮素的分析方法. 比较了单液滴液相微萃取和中空纤维液相微萃取两种萃取模式, 选择了单液滴液相微萃取作为3种多酚类化合物的液相微萃取模式. 考察了搅拌速度、萃取时间、料液相pH和料液相离子强度的影响. 鞣花酸、白藜芦醇和槲皮素的富集倍数分别为48.4、 79.4和155.8, 方法的线性范围为0.0050～5.0 μg/mL, 鞣花酸、白藜芦醇和槲皮素的检出限分别为0.015, 0.0020, 0.0080 μg/mL, 相对标准偏差分别为2.0%, 1.8%和1.7%. 用于实际样品葡萄汁的分析, 加标回收率在81.9%～102.3%之间.