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1.
Kinetics and products of photo-Fenton degradation of triazophos   总被引：6，自引：0，他引：6  
Triazophos is a contaminant of wastewater at manufacturing facilities, and remediative treatment may be needed. While toxicity and persistence limit the effectiveness of biological and physicochemical methods, photo-Fenton processes are promising. UV-Fenton and solar-Fenton processes were applied to degrade triazophos. The optimum parameters were 50 mmol/L H(2)O(2), 0.3 mmol/L FeSO(4), and pH 3.0. The decomposition of triazophos by a photo-Fenton process followed first-order kinemics. At 30 degrees C, the half-life of triazophos in a UV-Fenton process ranged from 9.1 min at 2.0 x 10(5) Lx to 27.3 min at 1.0 x 10(5) Lx. At 35 degrees C and with solar irradiation luminance, it ranged within 1.0 x 10(5) -1.2 x 10(5) Lx; the half-life of triazophos in the solar-Fenton process was 11.2 min. Five major degradation products, O,O-diethyl phosphorothioic acid, monoethyl phosphorothioic acid, phosphorothioic acid, 1-phenyl-3-hydroxy-1,2,4-triazole, and phenylsemicarbazine, were tentatively identified as their corresponding trimethylsilyl derivatives with a gas chromatography-mass spectrometer. The possible degradation pathway of triazophos was proposed. The results indicate the potential use of a solar-Fenton treatment for triazophos-contaminated water.  相似文献   

2.
The hydrolysis of triazophos was studied in buffered solutions in the range of pH 4-10 and in sodium hydroxide solutions with pH values up to 12. The results showed that the degradation of triazophos in the above solutions followed simple pseudo-first-order kinetics. At 35 degrees C, the rate constants in buffered solutions ranged from 0.0222 d(-1) at pH 4 to 0.5357 d(-1) at pH 10, and increased to 0.6251 h(-1) in 0.01 mol/L sodium hydroxide solution. The results also indicated that the base-catalysis was more important than acid-catalysis in the hydrolysis of triazophos. On the basis of the Arrhenius plot, the calculated activation energy (E(a)) and the frequency factor (A) for the hydrolysis of triazophos in buffered solution of pH 10 were 78.6 kJ/mol and 1.13 x 10(13) d(-1), respectively. Hydrolytic products of triazophos in buffered solutions of pH 4 and 10, as well as in sodium hydroxide solution of pH 11, were identified as their corresponding trimethylsilyl derivatives with a gas chromatography-mass spectrometer (GC-MS). The possible hydrolytic pathways of triazophos were also proposed.  相似文献   

3.
The validation of a liquid chromatographic procedure suitable for the determination of calcitriol and alfacalcidol in their respective formulations labeled to contain at least 0.25 micrograms drug per unit is described. The capsule content is diluted and chromatographed in 15-20 min on silica columns (5 micron) with a mobile phase of hexane-tetrahydrofuran-methylene dichloride-isopropanol (72 + 12 + 12 + 4, v/v) with detection at 254 nm. The calibration curve is linear. Recoveries of "spikes" averaged 101% with a standard deviation of 2%. Precision was better than 1.5%.  相似文献   

4.
The normal phase liquid chromatographic (LC) method for determination of trans- and cis-isomers of vitamin K1 (phylloquinone) in infant formula described here uses an Apex silica column, isocratic elution, and UV absorption detection at 254 nm. Vitamin K1 is extracted quantitatively from the product matrix by pretreating the as-fed liquid with concentrated ammonium hydroxide and methanol, and then extracting it with a 2:1 mixture of dichloromethane and isooctane. The extract is cleaned up by silica open-column chromatography and concentrated for LC analysis. For trans-vitamin K1, the method precision is less than or equal to 3.3% RSD (relative standard deviation), and the spike recovery is 98 +/- 4%. For cis-vitamin K1, the precision is less than or equal to 12% RSD, determined at levels near the detection limit, and the spike recovery is 95 +/- 9%. The detection limit is 0.3 ng for both isomers at signal/noise = 3.  相似文献   

5.
Light-induced formation of lipid peroxides in a water-in-oil emulsion based on purified rape-seed oil (80%) was found to increase with decreasing wavelength and to have the (apparent) quantum yields (1.1 +/- 0.1) x 10(-)(3) for 436 nm, (2.6 +/- 0.1) x 10(-)(3) for 405 nm, and (4.5 +/- 0.4) x 10(-)(3) for 366 nm irradiation, as determined after 12 h of exposure to monochromatic light of an approximate intensity of 10(18) quanta.min(-)(1).mL(-)(1) and related to total light absorption. Riboflavin (0.8 ppm) had no effect on lipid peroxidation, but photodegraded with a quantum yield ((1.5 +/- 0.3) x 10(-)(5) for 436 nm, (1.7 +/- 0.2) x 10(-)(5) for 405 nm and (1.39 +/- 0.09) x 10(-)(5) for 366 nm irradiation) independent of irradiation wavelength. beta-Carotene was only photodegraded to a minor extent, but protected riboflavin against photodegradation and the lipids against peroxidation for 436 and 405 nm irradiation (reduction in quantum yield three times for 4.5 ppm beta-carotene for lipid oxidation and more for riboflavin degradation), but not for 366 nm irradiation, where beta-carotene has an absorption minimum.  相似文献   

6.
Phototransformation of propiconazole in aqueous media.   总被引：2，自引：0，他引：2  
The photolysis of propiconazole in pure water, in water containing humic substances, and in natural water was investigated. The reaction rates were determined, and the main photoproducts were identified with the help of HPLC-mass spectrometry and by NMR. The quantum yield for direct photolysis was 0.11 +/- 0.01 at the maximum of absorption (269 nm). Photocyclization after HCl elimination and photohydrolysis of the cyclized intermediate were the main reaction pathways at 254 nm. By contrast, oxidation prevailed over dechlorination in simulated or natural solar light. Humic substances (10 mg x L(-)(1)) and naturally occurring chromophores contained in natural water enhanced the rate of propiconazole photodegradation in solar light. Half-life in June in Clermont-Ferrand (latitude 46 degrees N) was found to be 85 +/- 10 h in pure water and 60 +/- 10 h in natural water; showing that photodegradation of propiconazole in natural waters involves both direct photolysis and photoinduced reactions.  相似文献   

7.
Sucralose used as high potency sweetener in foods was determined in burfi, a milk-based confection produced in-house. Therefore planar chromatography was employed as a preferred method because of a reagent-free derivatization step. Sucralose was determined on HPTLC amino plates whose amino groups reacted with sucralose to fluorescent zones by just heating the plate after chromatography. Thus derivatization was simultaneously performed for 22 separations per plate, and with ease, over 300 runs can be performed within a day of labor. The within-run precision (%RSD) of sucralose determination in milk-based confection was 4.2% (n = 5), and the mean recovery 88% +/- 4.7% (n = 6). LOD via fluorescence measurement was 6 ng/band for standard solutions and 1 mg/kg for the milk-based matrix. According to European legislation, the limits for sucralose addition ranged between 10 and 3000 mg/kg for various foods and thus were fully met with this method. The fluorescence measurement at 366/>400 nm turned out to be slightly more robust and intense than the absorbance measurement at UV 254 nm. The stability of sucralose in milk-based confection was proved under the usual storage conditions at 5, 30, and 45 degrees C for up to 28 days. Potential hydrolysis products of sucralose caused by various modes of storing the confection were not observed up to 28 days.  相似文献   

8.
Phenolic compounds present in crude oil extracts from acai fruit ( Euterpe oleracea) were identified for the first time. The stability of acai oil that contained three concentrations of phenolics was evaluated under short- and long-term storage for lipid oxidation and phenolic retention impacting antioxidant capacity. Similar to acai fruit itself, acai oil isolates contained phenolic acids such as vanillic acid (1,616 +/- 94 mg/kg), syringic acid (1,073 +/- 62 mg/kg), p-hydroxybenzoic acid (892 +/- 52 mg/kg), protocatechuic acid (630 +/- 36 mg/kg), and ferulic acid (101 +/- 5.9 mg/kg) at highly enriched concentrations in relation to acai pulp as well as (+)-catechin (66.7 +/- 4.8 mg/kg) and numerous procyanidin oligomers (3,102 +/- 130 mg/kg). Phenolic acids experienced up to 16% loss after 10 weeks of storage at 20 or 30 degrees C and up to 33% loss at 40 degrees C. Procyanidin oligomers degraded more extensively (23% at 20 degrees C, 39% at 30 degrees C, and 74% at 40 degrees C), in both high- and low-phenolic acai oils. The hydrophilic antioxidant capacity of acai oil isolates with the highest phenolic concentration was 21.5 +/- 1.7 micromol Trolox equivalents/g, and the total soluble phenolic content was 1252 +/- 11 mg gallic acid equivalents/kg, and each decreased by up to 30 and 40%, respectively, during long-term storage. The short-term heating stability at 150 and 170 degrees C for up to 20 min exhibited only minor losses (<10%) in phenolics and antioxidant capacity. Because of its high phenolic content, the phytochemical-enriched acai oil from acai fruit offers a promising alternative to traditional tropical oils for food, supplements, and cosmetic applications.  相似文献   

9.
Heat-induced morphological change in myosin filaments was observed using atomic force microscope. The thickness of fixed native myosin filament was estimated to be 95 +/- 5 nm. When myosin filaments in 0.1 M NaCl at pH 6.0 were heated at 40, 55, and 70 degrees C for 10 min, the particulate structure appeared spirally on the surface of the filament at 40 degrees C, and the thickness of the filament was 75 +/- 10 nm. When myosin filaments were treated at 55 degrees C, several filaments were formed associated with side-by-side interaction through projected myosin heads to form a strand. The surface of the strand looked knobby. The thickness of thermally denatured filaments at 55 degrees C was 48 +/- 5 nm, and that of strands was about 80-110 nm, indicating the involvement of several filaments in a strand. The strands became to be rope-like at 70 degrees C, and the individual filaments in a strand were not distinguishable.  相似文献   

10.
Recent research suggests that blueberries are rich in total polyphenols and total anthocyanins. Phenolic compounds are highly unstable and may be lost during processing, particularly when heat treatment is involved. There is no systematic study available providing information on the fate of phenolic compounds during storage and how that affects their biological activity. We provide a systematic evaluation of the changes observed in total polyphenols (TPP), total anthocyanins (TACY), Trolox equivalent antioxidant capacity (TEAC), phenolic acids, and individual anthocyanins of blueberry extract stored in glass bottles and the ability of blueberry extract to inhibit cell proliferation. The extract was stored at different temperatures (-20 +/- 1, 6 +/- 1, 23 +/- 1, and 35 +/- 1 degrees C). Two cultivars, Tifblue and Powderblue, were chosen for the study. The recoveries of TPP, TACY, and TEAC in blueberry extract after pressing and heating were approximately 25, approximately 29, and approximately 69%, respectively, for both cultivars. The recovery of gallic acid, catechin, and quercetin was approximately 25%. Ferulic acid was not detected in the final extract in both Tifblue and Powderblue cultivars. The recovery of peonidin, malvidin, and cyanidin glycosides was approximately 20% in the final extract in both cultivars. Losses due to storage were less when compared with initial losses due to processing. At -20 degrees C, no statistically significant loss of TPP, TACY, and TEAC was observed up to 30 days (P < 0.05). At 6 degrees C storage, there was a significant loss observed from 15 to 30 days. Similar results were obtained at 23 and 35 degrees C (P < 0.05). There was retention of more than 40% of ellagic and quercetin after 60 days at 35 +/- 1 degrees C. Anthocyanins were not detected after 60 days of storage at 35 +/- 1 degrees C. Significant retention (P < 0.05) was obtained for malvidin (42.8 and 25.8%) and peonidin (74.0 and 79.5%) after 60 days of storage at 23 +/- 1 degrees C in glass bottles for Tifblue and Powderblue, respectively, when compared with other individual anthocyanins. A linear relationship was observed between TEAC values and total polyphenols or total anthocyanins. A cell viability assay was performed using HT-29 cancer cell lines and anthocyanins extracted from 30, 60, and 90 days of stored extract at 6 +/- 1 and 23 +/- 1 degrees C. A significant cell proliferation inhibition percentage was observed in 30 days, although this was reduced significantly after 30-90 days. These results suggest that heating and storage conditions significantly affect the phenolic compounds and their biological activities. Frozen and low temperature storage are suggested for blueberry extract in order to retain the bioactive components.  相似文献   

11.
Some iodoamino acids have been separated and determined by high pressure liquid chromatography on octadecylsilane reverse phase packing with a mobile phase consisting of methanol, potassium phosphate monobasic, and orthophosphoric acid at 44 degrees C. The method separates and quantitates mixtures of 3,5-diiodothyronine, liothyronine, isoliothyronine, and levothyroxine. The procedure provides an accurate, sensitive, and rapid estimation of decomposition and/or impurities in standards in approximately 30 min, at the less than 75 pmole level, using an ultraviolet detector at 254 nm.  相似文献   

12.
Bovine beta-lactoglobulin, genetic variant B, has been labeled with 2-(4'-maleimidylanilino)naphthalene-6-sulfonic acid through covalent attachment through the Cys-121 thiol group for the study of stepwise pressure denaturation of this whey protein by fluorescence spectroscopy. The labeling was performed under nondenaturing conditions with a factor of 5 excess of the fluorophore in dimethylformamide/water (1:10) to yield the whey protein highly labeled after chromatographic separation. MALDI-TOF mass spectroscopy confirmed labeling. The emission from the fluorophore, which is sensitive to the microenvironment, has been characterized for the labeled protein (aqueous pH 7.4 solution, 25 degrees C) and has a lambda(em,max) = 410 nm (lambda(ex,max) = 318 nm) with a fluorescence lifetime of 6.1 +/- 0.2 ns. Fluorescence anisotropy increases and fluorescence quantum yield (Phi(f) = 0.103 at 320 nm) decreases with increasing excitation wavelength. For increasing hydrostatic pressure, fluorescence quantum yield showed a minimum at approximately 50 MPa, corresponding to the pre-denatured "pressure-melted" state in which thiol reactivity previously was found to increase prior to reversible protein unfolding.  相似文献   

13.
A hazelnut-specific sandwich-type ELISA based on polyclonal antisera was developed for detection of hidden hazelnut protein residues in complex food matrixes. In the absence of a food matrix, extractable protein from different native and toasted hazelnuts was detected at rates of 94 +/- 13 and 96 +/- 7% applying standards prepared from native and toasted hazelnuts, respectively. From complex food matrixes, 0.001-10% of hazelnut was recovered between 67 and 132%, in average by 106 +/- 17%. Depending on the food matrix, hazelnut protein could be detected down to the ppb (ng/g) level. Intraassay precision was <6% for hazelnut >/= 0.001% and interassay precision was <15% for hazelnut >/= 0.01%. In 12 of 28 commercial food products without labeling or declaration of hazelnut components, between 2 and 421 ppm of hazelnut protein was detected, demonstrating a remarkable presence of potentially allergenic hazelnut protein "hidden" in commercial food products.  相似文献   

14.
A rapid, reliable method for the simultaneous determination of creatinine and pseudouridine is described. Both analytes were detected at an optimum wavelength of detection (262 nm), considering the relative levels present in bovine urine. Cimetidine was used as the internal standard and detected at its maximum wavelength of absorption (220 nm) on a separate channel. All three compounds were eluted within 15 min, using a 10 mmol/L phosphate buffer (pH 6.8)-methanol gradient on a C18 column. Creatinine data were found to be significantly dependent upon the pH of the sample. Recoveries of both analytes were above 96%. Lowest detectable levels of creatinine and pseudouridine were 0.28 nmol and 9.0 pmol, respectively. The use of internal standard resulted in a method with high precision (standard deviation of 1.42 mmol/L and 0.027 mmol/L for creatinine and pseudouridine), yet one that was simple and rapid.  相似文献   

15.
Molecular complexes based on proteins and ionic polysaccharides have considerable potential for encapsulation of functional food components, but their widespread utilization is limited because their structure is highly sensitive to pH and ionic strength. We have investigated the possibility of creating stable hydrogel particles by thermal treatment of protein (beta-lactoglobulin) and cationic polysaccharide (chitosan) mixtures. Mixed solutions of beta-lactoglobulin (0.5 wt %) and chitosan (0.1 wt %) were prepared at various pH's (3-8) and were heated (80 degrees C for 20 min). Prior to heating, the biopolymer mixtures formed molecular complexes at pH values where there was an electrostatic attraction between the protein and the polysaccharide: soluble complexes at pH 4.5; complex coacervates at pH 5.0 and 5.5; precipitates at pH>5.5. After heating, relatively small (d approximately 140 nm) and cationic (zeta>+20 mV) hydrogel particles were formed at pH 4.5, but much larger aggregates were formed at pH 5.0 and higher (d>1000 nm). The thermally treated hydrogel particles formed at pH 4.5 maintained their initial particle size when the pH was subsequently adjusted within the range pH 3-5, but they aggregated when the pH was adjusted to >pH 5 because of a reduction in the magnitude of their electrical charge. This study suggests that hydrogel particles can be formed by heating mixed protein-polysaccharide systems under controlled conditions. These hydrogel particles may be useful for encapsulation of functional food components.  相似文献   

16.
This study was undertaken to follow the kinetics of polyphenoloxidase (PPO), peroxidase (POD), and phenolic compounds during yam blanching at different temperatures and after drying and to identify by high-performance liquid chromatography (HPLC) the main phenolic compounds present in yam products. PPO activity was 50% higher in nonprocessed freeze-dried Florido (Dioscorea alata) than in nonprocessed freeze-dried Deba (Dioscorea rotundata). It decreased progressively during blanching. Forty-five percent of PPO activity remained after 50 min of blanching at 60 or 65 degrees C, whereas the POD activity dropped sharply to less than 20% of the initial activity after 10 min of blanching, whatever the blanching temperature. No anthocyanidins could be detected by HPLC at 520 nm in nonprocessed freeze-dried yam. Flavanols with a maximum absorption wavelength (lambda(max)) at 280 nm and cinnamic acid compounds with 320 nm lambda(max) were detected. Catechin was identified as the major flavanol with concentrations ranging from 0.26 to 0.41 microM g(-)(1) depending on cultivar. One cinnamic compound, ferulic acid, was identified and assessed in both cultivars (0.03-0.04 microM g(-)(1)). Total phenol, flavanol, and cinnamic contents decreased during blanching independently of temperature whereas some unresolved peaks were detected by HPLC in dried product. The latter was probably due to the consumption of coloring precursors and the appearance of polymerized or complex colored products.  相似文献   

17.
A simple and rapid method is presented for the liquid chromatographic assay of ascorbic acid, niacinamide, pyridoxine, thiamine, and riboflavin from a single chromatogram. Ion-pair chromatography with a reverse phase C18 cartridge in a radial compression system is used. Quantitation is excellent with a total analysis time of less than 20 min. A mobile phase of methanol-water (15 + 85) (0.005M heptanesulfonic acid) with 0.5% triethylamine at pH 3.6 and a flow rate of 2.0 mL/min gives the most satisfactory separation of the 5 water-soluble vitamins. By using 2 detectors in series set at different wavelengths and sensitivities, all 5 vitamins, with peak heights on scale, can be measured from a single injection; peak elution order is ascorbic acid, niacinamide, pyridoxine, thiamine, and riboflavin. Ascorbic acid is measured at 254 nm and the other vitamins, at 280 nm. The amount of amine modifier in the mobile phase is critical to the separation of niacinamide and pyridoxine. Recoveries of 5 water-soluble vitamins from spiked placebos were in the range of 98.2-102.0%. Confidence limits, +/- 3 SD, were in the range of 1.0-5.4%. Overall, the results obtained using the liquid chromatographic method show excellent agreement with manual methods and automated analysis.  相似文献   

18.
Processed fruits and vegetables have been long considered to have lower nutritional value than their fresh commodities due to the loss of vitamin C during processing. This research group found vitamin C in apples contributed < 0.4% of total antioxidant activity, indicating most of the activity comes from the natural combination of phytochemicals. This suggests that processed fruits and vegetables may retain their antioxidant activity despite the loss of vitamin C. Here it is shown that thermal processing elevated total antioxidant activity and bioaccessible lycopene content in tomatoes and produced no significant changes in the total phenolics and total flavonoids content, although loss of vitamin C was observed. The raw tomato had 0.76 +/- 0.03 micromol of vitamin C/g of tomato. After 2, 15, and 30 min of heating at 88 degrees C, the vitamin C content significantly dropped to 0.68 +/- 0.02, 0.64 +/- 0.01, and 0.54 +/- 0.02 micromol of vitamin C/g of tomato, respectively (p < 0.01). The raw tomato had 2.01 +/- 0.04 mg of trans-lycopene/g of tomato. After 2, 15, and 30 min of heating at 88 degrees C, the trans-lycopene content had increased to 3.11+/- 0.04, 5.45 +/- 0.02, and 5.32 +/- 0.05 mg of trans-lycopene/g of tomato (p < 0.01). The antioxidant activity of raw tomatoes was 4.13 +/- 0.36 micromol of vitamin C equiv/g of tomato. With heat treatment at 88 degrees C for 2, 15, and 30 min, the total antioxidant activity significantly increased to 5.29 +/- 0.26, 5.53 +/- 0.24, and 6.70 +/- 0.25 micromol of vitamin C equiv/g of tomato, respectively (p < 0.01). There were no significant changes in either total phenolics or total flavonoids. These findings indicate thermal processing enhanced the nutritional value of tomatoes by increasing the bioaccessible lycopene content and total antioxidant activity and are against the notion that processed fruits and vegetables have lower nutritional value than fresh produce. This information may have a significant impact on consumers' food selection by increasing their consumption of fruits and vegetables to reduce the risks of chronic diseases.  相似文献   

19.
For the first time, a cytosolic carotenoid cleavage enzyme isolated from quince (Cydonia oblonga) fruit is described. The enzyme was partially purified by using centrifugation, acetone precipitation, ultrafiltration (300 kD, 50 kD), isoelectric focusing (pH 3-10), and sodium dodecyl sulfate polyacrylamide gel electrophoresis (7.5%). In this way, an enzymatically active protein fraction was obtained that contained three similar proteins, all exhibiting molecular weights in the range of 20 kD. Using beta-carotene as substrate, the enzyme activity was detected spectrophotometrically at a wavelength of 505 nm. The time constant of the reaction was 8.2 min, the Michaelis constant (K(m)) was 11.0 micromol x L(-1), and the maximum velocity (v(max)) was 0.083 micromol x L(-1) x min(-1) x mg(protein)(-1). The optimum temperature was above 50 degrees C.  相似文献   

20.
Polyphenol oxidase (PPO) and peroxidase (POD) were extracted from two different varieties of melon ( Cucumis melo L. cantalupensis cv. Charentais and C. melo L. inodorus cv. Amarillo) and characterized using reliable spectrophotometric methods. In both cases the enzymes followed Michaelis-Menten kinetics, showing different values of kinetics parameters between the two cultivars: K m = 7.18 +/- 0.70 mM ('Charentais') and 6.66 +/- 0.20 mM ('Amarillo') mM; V max = 7.93 +/- 0.35 units/min ('Charentais') and 13.82 +/- 0.37 units/min ('Amarillo'), relative to PPO; K m = 24.0 +/- 2.10 mM ('Charentais') and 5.05 +/- 0.19 mM ('Amarillo') mM; V max = 344.83 +/- 10.32 units/min ('Charentais') and 80.64 +/- 2.01 units/min ('Amarillo'), relative to POD. Optimum pH for PPO was 7.0 for 'Charentais' and 7.5 for 'Amarillo, whereas it was 4.5 for both cultivars relative to POD. Melon PPO had maximum activity at 60 degrees C in both 'Charentais' and 'Amarillo' cultivars, whereas POD maximum activity was found at 45 degrees C in 'Charentais' and at 25 degrees C in 'Amarillo'. POD from both cultivars showed higher thermolability compared with PPO, losing >90% of relative activity after only 5 min of incubation at 70 degrees C. POD's activation energy was much higher than that of PPO (Delta E (#) = 86.3 and 160.6 kJ mol (-1) for 'Charentais' and 'Amarillo', respectively). PPO and POD activities from both cultivars showed a decreasing pattern as sugar concentration in the assay medium increased, except in POD extract from 'Charentais', which maintained its activity in the presence of high d-glucose concentration (up to 5 M). Changes in L*, a*, b*, chroma, and hue angle values were chosen to describe the browning development in the samples during storage at 5 degrees C. A slight decrease in L* value and a more marked reduction of a* value were noted in both cultivars above all at the end of storage period. POD activity during storage at 5 degrees C was highly correlated with changes of parameters a*, b*, chroma, and hue angle ( r (2) from 0.82 to 0.97) for cultivar 'Charentais'. According to these results, only POD activity seemed to be involved in browning of minimally processed melon.  相似文献   

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