Calcium Alginate Foams Prepared by a Microfluidic T-Junction System: Stability and Food Applications

Highly porous alginate foams were prepared via a novel route in which highly viscous alginate solutions were bubbled using a microfluidic T-junction device. The relationship between bubble size and bubbling conditions such as air pressure and solution flow rate was studied, and the ability of the T-junction setup to generate monodisperse microbubbles (mean diameter, ～154 μm) and produce porous foams was systematically investigated. The foams were characterised by optical and scanning electron microscopy. Foams of varying lengths (12–45 mm) were successfully prepared using this technique, with an average density of ～235 kg/m³. The pore diameter within the foams was determined by microscopy to be in the range of 600 nm–200 μm with a mean diameter of ～31 μm. It was concluded that porosity in the foam (>90%) can be varied depending on the initial bubble size. Thus, a possible production method of stable highly porous solid foams for exploitation in food and bioprocess technologies is presented by which products can be made to different sizes.     

A simple and efficient ultrasonic-assisted extraction procedure combined with UV-Vis spectrophotometry for the pre-concentration and determination of folic acid (vitamin B9) in various sample matrices

A simple and efficient ultrasonic-assisted extraction (UAE) procedure has been proposed for the pre-concentration of (2S)-2-[(4-{[(2-amino-4-hydroxypteridin-yl)methyl]amino}phenyl)formamido]pentanedioic acid (folic acid) in vegetables, pharmaceuticals and foods prior to determination at 540 nm using UV-Vis spectrophotometry. The method is based on hydrophobic ternary complex formation of folic acid with silver ions in the presence of cetyltrimethylammonium bromide (CTAB) as a sensitivity enhancer counter ion at pH 7.0, and then extraction into a micellar phase of polyethylene glycol monoalkyl ether (Genapol X-080). The impacts on the extraction efficiency and complex formation of analytical parameters such as sample pH, concentration of silver, concentration of surfactants and extraction time, ultrasonic time and sample volume, were investigated and optimised in detail. The matrix effect on the pre-concentration and determination of folic acid was investigated, and it was observed that the proposed method was highly selective against possible matrix co-extractives. Under optimised conditions, a good linear relationship between the analytical signal and folic acid concentration was obtained in the range of 0.6–180 μg l^?1 with a detection limit of 0.19 μg l^?1 and quantification limit of 0.63 μg l^?1. The applicability was evaluated using samples fortified at different concentration levels, and recoveries higher than 94.1% were obtained. The precision as the percent relative standard deviation (RSD%) was in range of 2.5–3.8% (10 and 40 μg l^?1, n = 5). The proposed method was validated by analysis of two standard reference materials (SRMs) and various real samples, and satisfactory results were obtained.     

Simultaneous determination of aspartame,acesulfame-K,saccharin, citric acid and sodium benzoate in various food products using HPLC–CAD–UV/DAD

A newly developed method for simultaneous determination of aspartame, acesulfame-K, saccharin, citric acid and sodium benzoate in various diet supplements and non-alcoholic beverages in a single run is presented. The analytes were analysed by high-performance liquid chromatography coupled to a charged aerosol (Corona CAD) and ultraviolet–diode array detectors simultaneously connected in series. Mass spectrometer MicrOTOF-QII from Bruker Daltonik (Bremen, Germany) was used to obtain the mass spectra for peak identifications. The method was validated using a Thermo Hypersil Gold-C18 column packed with 5 μm shell particles (150 × 4.6 mm) and methanol–water with 0.05 % TFA gradient mobile phase at a flow rate of 0.80 mL/min. The elaborated method was validated for linearity, precision and accuracy. The analytical results obtained in the validation study were highly satisfying; the recoveries for the analytes studied ranged between 98.1 and 101 % and the precision values from 0.11 to 1.73 %. By these procedures, the three sweeteners (aspartame, acesulfame-K and saccharin), citric acid and sodium benzoate could be well separated and quantitatively determined in varied food products. Hundred millilitres of soft drinks contained on average 5.50 mg of aspartame, 6.38 mg of saccharin, 8.94 mg of acesulfame-K, 9.05 mg of sodium benzoate and 111 mg of citric acid. Citric acid was the most abundant additive in all the samples analysed except for table sweeteners, and its highest concentration was determined in diet supplements, i.e. 347 mg/g. The percentage of adequate daily intake realisation in case of all additives is lower than 10 %, except for sodium benzoate in isotonic drinks (10.1 %).     

Removal of Cd(II) ions by oxidized coconut coir

Biosorption potential of oxidized coconut coir (OCC) for removal of Cd(II) from aqueous medium at batch and column level was studied. Lignin and cellulose groups of coir were modified to acidic groups. Optimum biosorption was observed at pH 6. Isotherm data revealed that Langmuir gives best fit for experimental results with maximum adsorption capacity of 12.35 mg/g compared to unmodified coconut coir (5.29 mg/g). The column experiments were conducted as a function of flow rate, bed height, and influent Cd(II) concentration. Biosorption has best performance at 10 mg/L inlet concentration, 5 ml/min flow rate and 7 cm bed height.     

Simultaneous Determination of Flumequine and Oxolinic Acid Residues in Aquatic Products Using Pressurized Capillary Electrochromatography

A rapid method for detection of flumequine (FQ) and oxolinic acid (OA) residues from fish tissues was established using pressurized capillary electrochromatography (pCEC). Residual FQ and OA were extracted from fish tissue samples with acidified acetonitrile and purified on an Oasis HLB C₁₈ solid-phase extraction column. The extract was then analyzed by pCEC with the mobile phase (pH?=?3) consisting of acetonitrile and 15 mM ammonium acetate (45: 55, v/v, respectively) at the flow rate of 0.07 mL/min, detection wavelength of 324 nm, and applied voltage of ?10 kV. Baseline separation of FQ and OA was achieved in 10 min; both drugs showed good linearity in the range of 0.2–5 μg/mL. The recoveries of FQ and OA were between 82 and 92 % (relative standard deviation?=?3.63–5.96). The limits of detection for FQ and OA were 0.1 and 0.08 mg/kg, respectively.     

Application of alginate and gelatin-based edible coating materials as alternatives to traditional coating for improving the quality of pastirma

This research was conducted to study the efficacy of sodium alginate and gelatin coating materials in improving the quality of pastirma. Pastirma was coated with traditional, alginate or gelatin coatings, stored at 4 °C for 4 weeks and examined weekly. Alginate and gelatin coated-pastirma revealed lower TBARS values which was within the acceptable limit (0.67 and 0.86 mg/kg) until the end of storage, however, the TBARS values of traditionally coated pastirma reached 1.33 by the end of storage. Edible coating delayed respiration rate with improvement of the color when compared with traditionally coated one. Oxygen concentration increased from 4.21 mg/kg/h in traditionally coated pastirma to 12.56 and 9.79 in alginate and gelatin coated ones, respectively. Meanwhile, CO₂ concentration decreased from 10.40 mg/kg/h in traditionally coated pastirma to 4.89 and 6.07 mg/kg/h in alginate and gelatin coated ones, respectively. Moreover, a distinct improvement in all sensory attributes has been observed.     

高效液相色谱-质谱联用测定婴幼儿配方食品中叶酸的含量

建立了婴幼儿配方食品中叶酸含量的高效液相色谱-质谱联用测定方法。采用C18色谱柱(4.6mm×250mm,5μm)进行分离,以5 mmol/L乙酸铵(含0.1%甲酸)溶液-甲醇为流动相梯度洗脱,柱温25℃,流速1.0 mL/min,进样量20μL,柱后分流比为1∶3,质谱采用多离子反应监测(MRM)方式进行检测,正离子模式,定量离子为m/z442.0→295.2。叶酸在0.001~2.500μg/mL的范围内线性关系良好(r=0.9989),该方法相对标准偏差(RSD)为2.6%~6.0%,回收率为83.9%~104.0%,检出限(S/N=3)和定量限(S/N=10)分别为1.0 ng/mL、3.3 ng/mL。该方法操作简便、灵敏度高、重复性好,可用于婴幼儿配方食品中叶酸的测定。     

Determination of Phenolic Compounds in Artichoke,Garlic and Spinach by Ultra-High-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry

Phenolic compounds were determined in artichoke (Cynara scolymus), garlic (Allium sativium) and spinach (Spinacia oleracea) using a single method based on simple extraction and ultra-high-performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry (UHPLC-QqQ-MS/MS). Several compounds belonging to different families, such as phenolic acids, isoflavones, flavones and flavonols, were determined. The analytical procedure was validated in all the matrices, obtaining recoveries ranging from 60 to 120 % with reproducibility values (expressed as relative standard deviations (RSDs)) lower than 26 %. Limits of quantification (LOQs) were always equal to or lower than 50 μg/kg, except to kaempferol and its glucosides in spinach (LOQs?=?75 μg/kg). Artichoke showed higher concentration of phenolic compounds (837.2 mg/kg dry weight (DW)) than garlic (26.5 mg/kg DW) or spinach (64.5 mg/kg DW). Apigenin 7-O-glucoside (from 147.0 to 722.7 mg/kg DW) was found to be the major flavonoid in all samples of artichoke investigated, while chlorogenic acid, whose concentration ranged from 37.8 to 734.7 mg/kg DW, is the major phenolic acid in this matrix. Regarding garlic, caffeic acid (from 1.7 to 28.3 mg/kg DW) and quercetin (from 9.0 to 18.9 mg/kg DW) were the compounds detected at higher concentrations, although in general the total content was very low in relation to other matrices. In relation to spinach, ferulic acid was the major phenolic compound, and its concentration ranged from 18.0 to 41.4 mg/kg DW.     

Molecularly Imprinted Polymer as Sorbent for Solid-Phase Extraction Coupling to Gas Chromatography for the Simultaneous Determination of Trichlorfon and Monocrotophos Residues in Vegetables

In this study, a molecularly imprinted polymer (MIP) was prepared using the mixture of trichlorfon and monocrotophos as the mixed template. The imprinted polymer was characterized and exhibited good recognition ability and fast adsorption–desorption dynamic toward the trichlorfon and monocrotophos. Using this imprinted polymer as sorbent, a new method of molecularly imprinted solid-phase extraction coupled to gas chromatography for the simultaneous determination of two organophosphate pesticides residues was developed. Under optimal condition, the linear range was 0.005–10.0 mg/l. At a loading flow rate of 2.0 ml/min for loading 100 ml, the detection limits were 0.28 μg/l for trichlorfon and 0.090 μg/l for monocrotophos, the peak area precision (RSD) for five replicates was 4.23–4.50 %. The blank rape samples spiked with two organophosphate pesticides at 0.05 and 0.1 mg/l levels were determined by this method with recoveries ranging from 89.41 % to 95.12 %. Moreover, this method was successfully applied to the quantitative detection of the trichlorfon and monocrotophos residues in leek samples.     

Use of Experimental Design and Artificial Neural Network in Optimization of Capillary Electrophoresis for the Determination of Nicotinic Acid and Nicotinamide in Food Compared with High-Performance Liquid Chromatography

A simple capillary electrophoresis (CE) method for the analysis of nicotinic acid (NA) and nicotinamide (NAM) was developed. Important experimental factors were optimized with response surface approach. Statistical models were constructed by Box–Behnken design as well as artificial neural network using the three selected variables (buffer concentration, sodium dodecyl sulfate (SDS) concentration, and voltage). Optimum separation conditions obtained were 10 mM sodium borate/10 mM SDS buffer, pH 9.0, 25 kV applied voltage, and UV detection at 210 nm. Linear relationships between peak-area and the content of the analytes were obtained in the concentration range (1.0–100 μg mL^?1), and the detection limit was less than 0.15 μg mL^?1. The method was applied to the determination of NA and NAM in different kinds of samples with satisfactory separation in less than 5 min. In addition, a comparison with high-performance liquid chromatography demonstrated that the developed CE method was comparable with regard to linearity, sensitivity, precision, and accuracy, but the analysis time and reagent consumption for CE were decreased significantly.     

Continuous production of wine vinegar in bubble column reactors of up to 60-litre capacity

This paper describes the development of a continuous acetic acid fermentation process for the production of wine vinegar in bubble column reactors of up to 60 l capacity. To determine appropriate fermentation conditions a study of the influence of residual ethanol concentration, inlet flow rate and aeration was carried out using a 6-l laboratory reactor, white table wine as fermentation medium, a temperature of 30 °C and an air flow rate of 0.125 min^-1 (vvm). The concentration of acetic acid obtained in the continuous wine vinegar production ranged from 91 g/l at 28.6 ml/h to 28 g/l at 154.1 ml/h by increasing the inlet flow rate. As expected, the biomass decreased as well, from 208 mg/l to 106 mg/l. The maximum acetification rate was observed in the range 85-110 ml/h, corresponding to a value of about 1.1 g/l/h. A further increase in the flow rate produced a slight decrease in the acetification rate. Best yields, between 94.5 and 94.7%, were obtained in the flow rate range of 60-75 ml/h. The acetification rate was improved only by about 10% by increasing the aeration from 0.125 to 0.250 min^-1. The continuous wine vinegar production was scaled up from the laboratory fermentor to a 60-l pilot acetator. During the steady state (residential time >6), with an inlet flow rate of 950 ml/h, temperature of 30 °C and aeration of 0.250 min^-1, the following parameters were obtained: acetic acid concentration 72 g/l, overall productivity 1.41 g/l/h and yield 94.2%.     

高效液相色谱法测定保健食品多维康胶囊中叶酸的含量

目的建立高效液相色谱法(high performance liquid chromatography,HPLC)测定多维康胶囊中叶酸含量的方法。方法采用C₁₈(150mm×4.6mm,5μm)色谱柱,以磷酸二氢钾-甲醇溶液为流动相,流速0.8 mL/min,检测波长254 nm,柱温30℃,进样体积10μL。结果叶酸的线性关系良好,相关系数为1.000;方法检出限为0.034μg/mL,定量限为0.091μg/mL;方法平均加标回收率为98.80%~104.17%,平均相对标准偏差为0.02%。结论该方法操作简单,灵敏度高,可作为保健食品多维康胶囊中叶酸的测定方法。     

Influence of Spray-Drying Conditions on Physical and Morphological Characteristics of Microencapsulated Benzoic Acid

Benzoic acid is widely used as a preservative in the food and feed industry, and microencapsulation is important in the application of this ingredient in various food products. The objective of this work was to evaluate the effect of benzoic acid concentration and drying air temperature on the physical characteristics of powders produced by spray drying, using maltodextrin and modified starch as the wall materials. A rotatable central composite design was used; the independent variables were inlet air temperature (145–180 °C) and benzoic acid concentration (2–10 %, m/m). Maximum yield was obtained when higher concentrations of benzoic acid and higher inlet air temperatures were applied. The highest microencapsulation efficiency was reached at intermediate temperatures (160 °C) and low concentration of benzoic acid. The particles size (D _[4,3]) ranged from 24.99 to 29.52 μm and, in general, presented amorphous structure, spherical shape with rough surfaces and had no cracks The optimum condition, considering all the response variables together, was drying air temperature 169 °C and benzoic acid concentration 6 % (m/m). Under these conditions, the particles presented solubility of 75.96 g/100 g and wettability of 56.8 s/g. Moreover, the process showed microencapsulation efficiency of 76.77 g/100 g and yield of 40.1 %. Spray drying was considered a potential process to provide microencapsulated benzoic acid.     

Optimization of Focused Ultrasound Extraction and Supercritical Fluid Extraction of Volatile Compounds and Antioxidants from Aromatic Plants

In this work, we have accomplished the optimization of focused ultrasound extraction and supercritical fluid extraction (SFE) of volatile oils and phenolic compounds from aromatic plants such as rosemary, oregano, and chamomile. The response surface analysis was the overall procedure to tackle this work. On the one hand, the focused ultrasound extraction method of volatile compounds was studied based on the use of cyclohexane as extractant (chamomile required cyclohexane:isopropanol (95:5)), and three parameters were optimized (cycles, amplitude, and time) for each plant. The quantification of the volatile compounds was performed by means of GC?×?GC-MS analysis and the volatile oil concentration rounded 10–310 μg/g for the oregano; 7–2,920 μg/g for the rosemary, and 0.8–244.2 mg/g for the chamomile. In the SFE method, four parameters were studied (oven temperature, pressure, CO₂ flow, and EtOH?%). The total polyphenol content was determined by Folin–Ciocalteu obtaining values from 1,000 to 12,000 mg gallic acid equivalent (GAE)/g plant. The antioxidant capacity was measured by Trolox equivalent antioxidant capacity obtaining values from 1.1 to 46.7 μmol Trolox equivalent/g plant.     

The UPLC–ESI–QqQLIT–MS/MS method for quantitative determination of phytochemicals in ethanolic extracts of different parts of eight Ficus species: Development and validation

Ficus and validation of the ultra performance liquid chromatography–electrospray ionization hybrid triple quadrupole–linear ion trap–tandem mass spectrometry (UPLC–ESI–QqQ_LIT–MS/MS) method in a multiple-reaction monitoring (MRM) mode for the quantitative determination of 19 phytochemicals. The chromatographic separation of targeted phytochemicals was performed using the Waters ACQUITY UPLC BEH? C18 column (1.7 μm, 2.1 mm × 50 mm) with 0.1% formic acid with water and acetonitrile as a mobile phase at a flow rate of 0.25 mL/min. The validation parameters showed the overall recoveries from 95.78?101.44% (RSD ≤ 3.25%), precision (intra-day: RSD ≤ 2.96%; inter-day: RSD ≤ 2.89%), linearity (R² ≥ 0.9982), limit of detection (8.60 × 10^–10?2.18 × 10^–6 mg/mL), and the limit of quantitation (2.60 × 10^–9–6.63 × 10^–6 mg/mL) in the concentration range from 0.5 to 1000 × 10^–6 mg/mL. This method was successfully applied in ethanolic extracts of different parts (fruits, leaves, and barks) of selected eight Ficus species. Quinic acid was predominant followed by rutin and chlorogenic acid among the studied nineteen phytochemicals. Ficus benjamina showed the maximum total content in fruits and leaves. The UPLC–ESI–QqQ_LIT–MS/MS method combined with principal component analysis (PCA) was successfully used for Ficus species discrimination on the basis of the contents of 15 compounds. The UPLC–ESI–QqQ_LIT–MS/MS method combined with PCA could be used for quality control.     

高压电场制备W/O/W复乳微囊的试验研究

为探索水溶性物质微囊化新方法,利用高压电场微胶囊成型装置制备W/O/W型微囊,内水相为蒸馏水,油相为液体石蜡,外水相为海藻酸钠溶液。研究了电压、液面距、推进速度、初乳/外相水溶液、海藻酸钠浓度对微囊粒径的影响。结果表明:在成囊范围内,电压、液面距和外水相海藻酸钠溶液浓度对微囊的粒径有较为显著的影响。在电压3.15～4kV,液面距2.5～10cm,海藻酸钠浓度0.6%～1.2%条件下,可以制得微囊粒径范围为50～1000μm之间,大小均匀的复乳微囊。     

A New Simplified and Stability Indicating Liquid Chromatography Method for Routine Analysis of Isoflavones Aglycones in Different Complex Matrices

In this work, a stability indicating method for routine analysis of isoflavones in different matrices was developed and validated. In order to simplify the analytical method, the glycosides were previously hydrolyzed to the corresponding aglycone forms. The separation of all isoflavone aglycones was achieved in 23 min, with a total time of analysis of 30 min, using trifluoroacetic acid 0.1 % (v/v) and acetonitrile:trifluoroacetic acid (100:0.01, v/v) as mobile phase. The LC method specificity was evaluated by the analysis of isoflavone standards submitted to acidic, alkali, neutral, oxidative, and photolytic stress conditions. The isoflavones degraded in alkali at 60 °C or in alkali under ulraviolet C (UVC) radiation, forming, in both conditions, three degradation products D1, D2, and D3 which were analyzed by liquid chromatography mass spectroscopy (LC-MS/MS). The method showed linearity higher than 0.999 with the concentration ranged from 0.1 to 10 μg ml^-1 for all isoflavone aglycones. The limits of quantitation obtained using calibration curves were from 0.28 to 0.37 μg ml^-1 and the intermediary precision at three levels (2, 6, and 10 μg ml^-1) showed RSD values between 0.03 and 0.25 %. After the performed validation, the LC method was applied to compare the isoflavone aglycones content in three different matrices: Glycine max beans, Glycine max dry extract, and isoflavone aglycone loaded nanoemulsion. The repeatability data showed RSD values between 0.02 and 1.41 % and the intermediary precision at three levels showed RSD values between 0.05 and 1.99 %. The recovery data of the isoflavone aglycones standards in the matrices at three levels were between 90.74 and 106.43 %.     

陶瓷覆聚乙烯醇——海藻酸钠膜固定化糖化酶的研究

用陶瓷颗粒吸附糖化酶后,再以不同配比的聚乙烯醇-海藻酸钠复合溶胶覆膜,分别对固定化条件、米氏常数、酶活残留率进行了研究,结果表明:陶瓷颗粒聚乙烯醇复合溶胶固定化糖化酶的条件是:聚乙烯醇:海藻酸钠配比为6∶4,溶胶浓度为7%,固化时间为120min。米氏常数为60.17mg/mL,酶活残留率为78%;陶瓷颗粒覆海藻酸钠复合溶胶固定化糖化酶的条件是:海藻酸钠∶聚乙烯醇配比是8∶2,溶胶浓度为1.5%,固化时间为90min。米氏常数为35.5mg/mL,酶活残留率为38%。     

Simultaneous Determination of Quercetin,Rutin, Naringin,and Naringenin in Different Fruits by Capillary Zone Electrophoresis

A fast and reliable capillary zone electrophoretic (CZE) method has been developed for the simultaneous determination of four fruit flavonoids using photodiode array (PDA) detector. The effects of CE parameters including concentration and pH of the running buffer, voltage, and injection time were optimized. Under the optimized conditions, all flavonoids were well determined in a 10 mM borate buffer of pH 8.5 within 10 min at an applied voltage of 25 kV. Naringin, naringenin, and quercetin were found to have linear response in the range of 3.12–200 μg/mL whereas rutin’s response was linear from 6.25 to 200 μg/mL. LOD was found to be 0.406, 0.314, 0.582, and 0.333 μg/mL and LOQ 1.355, 1.046, 1.941, and 1.11, respectively. Relative standard deviations (RSD) were found to be less than 3 % for both migration time and peak height which shows long-term stability and good reproducibility of the developed method. The method was successfully applied for the simultaneous determination of flavonoids from various fruit juice samples.     

利用弱碱性阴离子交换树脂从脱脂米糠中制取植酸的研究

以脱脂米糠为原料,通过酸浸、离子交换吸附、洗脱、精制、浓缩过程利用D318型弱碱性阴离子交换树脂制得植酸。试验结果表明,D318型阴离子交换树脂从脱脂米糠植酸粗溶液中吸脱植酸的最佳工艺条件为:吸附液浓度为10 mg/ml,吸附液流速为1.0 ml/min,NaOH洗脱液的流速为2.0 ml/min,NaOH洗脱液浓度为1.5 mol/L,操作温度为45℃,pH值为2.5左右。