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Microwave Assisted Solvent-free Synthesis of 1-phenyl-1, 2-dihydro-3H-naphtho[1, 2-e][1, 3]oxazin-3-one Catalyzed by FeCl3 微波辅助下FeCl3催化1-苯基- 1,2 -二氢- 3h -萘[1,2 -e][1,3]恶嗪-3-one的无溶剂合成
IF 5.6 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2019-09-01 DOI: 10.33945/SAMI/CHEMM.2019.5.1
Saeid Taghavi Fardood, A. Ramazani, M. Ayubi, Farzaneh Moradnia, Shahin Abdpour, Reza Forootan
Three-component coupling of 2-naphthol, aldehydes, and urea has been accomplished in the presence of FeCl3 under microwave irradiation and solvent-free conditions to afford the corresponding synthesis of 1-phenyl-1, 2-dihydro-3H-naphtho[1,2-e][1,3]oxazin-3-onederivatives in excellent yields. It is a promising catalyst for the microwave-assisted reaction providing high product yield in a short period.
在FeCl3存在下,在微波辐射和无溶剂条件下,完成了2-萘酚、醛和尿素的三组分偶联,从而以优异的收率合成了1-苯基- 1,2-二氢- 3h -萘[1,2-e][1,3]恶嗪-3- 1衍生物。它是一种很有前途的微波辅助反应催化剂,在短时间内具有较高的产物收率。
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引用次数: 4
Metal Free Synthesis of Organosulfur Compounds Employing Eosin Y as Photoredox Catalyst 以伊红Y为光氧化还原催化剂的无金属有机硫化合物合成
IF 5.6 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2019-09-01 DOI: 10.33945/SAMI/CHEMM.2019.5.3
F. Mangi, F. Sattar, Canzhong Lu
The organosulfur compounds are an important class of compounds with extensive pharmaceutical and synthetic concern as well as a prominent role in the living system. The development of effective methods for the introduction of sulfur atom into the carbon framework remains an eternal challenge, as most of the accounted process needs tenacious conditions. Owing to its economical and eco-friendly nature, eosin Y has emerged as a promising alternate to the transition metal catalyst in numerous organic transformations comprising C-H functionalization. The current work aims at a direct, efficient and single step synthetic route for the construction of thioethers, through oxidative coupling of the reaction partners facilitated by eosin Y as an organo photoredox catalyst.  The use of inexpensive and non-toxic dye, convenient reaction conditions, simple work-up procedure, and good to excellent yields are the advantages of this approach.
有机硫化合物是一类重要的化合物,具有广泛的药用和合成意义,在生命系统中具有突出的作用。开发将硫原子引入碳框架的有效方法仍然是一个永恒的挑战,因为大多数计算过程需要顽强的条件。由于其经济和环保的性质,伊红Y已成为过渡金属催化剂的一个有前途的替代品,在许多有机转化包括碳氢化合物功能化。目前的工作旨在通过伊红Y作为有机光氧化还原催化剂促进反应伙伴的氧化偶联,直接,高效,一步合成硫醚的合成路线。该方法的优点是使用廉价无毒的染料,反应条件方便,后处理程序简单,收率高。
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引用次数: 1
Synthesis of Pectin Graft Drug to Treatment the Wounds and Inflammations 果胶移植治疗创面炎症药物的合成
IF 5.6 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2019-09-01 DOI: 10.33945/SAMI/CHEMM.2019.5.10
F. M. Ali, Hameed M. Ahmed
This idea of this work included preparation new adhesive drug polymers to treatment the wounds and inflammations, new drug polymers were prepared as bio adhesive, which have high viscosity and treatment the wounds by the adhesion of both ends of the wound when it put as well as the speed of the treatment of external inflammation, because it remains inherent to the position of injury fast time, because of the property for it viscosity. A new bio adhesive polymer was prepared by modification of Pectin structure with acrylic acid (P1) as a spacer by using ceric ammonium nitrate (CAN) as an initiator, and new graft copolymer was substituted with amino drugs such as amoxicilli produced amide polymer. This design carries controlled delivery of therapeutic agents which could release the entrapped drug over an extended period of time due to its biodegradable, nontoxic and slow digesting nature. All prepared adhesive drug polymers were characterized by FTIR, 1H-NMR spectroscopes, thermo gravimetric analysis TGA and DSC were studied. intrinsic viscosities and physical properties of all prepared polymers were measured, biological activity was studied for all adhesive drug polymers  this new adhesive drug biological polymers were applied on different infected mice and wounds, It gave outstanding results and compliance mice infected with a full recovery by a short period of time.  The prepared drug copolymer was analyzed in different pH values at 37 °C in vitro study and controlled drug release was compared at zero time and after three days. The rate of hydrolysis in basic medium was found higher than acidic medium. It was concluded that modified drug release with extended drug action via slow release and in vivo performance was noted to be promising.
本工作的思路包括制备新型黏附药物聚合物来治疗伤口和炎症,将新型药物聚合物制备为生物黏附剂,它具有很高的黏附性,在伤口放置时通过伤口两端的黏附以及治疗外部炎症的速度来治疗伤口,因为它在损伤位置上保持固有的快时间,因为它的黏附性。以硝酸ceric铵(CAN)为引发剂,以丙烯酸(P1)为间隔剂对果胶结构进行改性,制备了一种新型的生物胶粘剂聚合物,并将其与氨基药物如阿莫西利生产的酰胺聚合物取代。由于其可生物降解、无毒和缓慢消化的特性,这种设计可以控制治疗药物的递送,可以在较长时间内释放被包裹的药物。采用红外光谱(FTIR)、核磁共振(1H-NMR)、热重分析(TGA)和差热分析(DSC)对所制备的黏附药物聚合物进行了表征。测定了所制备聚合物的特性粘度和物理性能,研究了所有黏附药物聚合物的生物活性。将这种新型黏附药物生物聚合物应用于不同感染小鼠和伤口上,效果显著,依从性好,感染小鼠在短时间内完全恢复。制备的药物共聚物在37℃不同pH条件下进行体外研究,并在0时和3天后进行药物控释比较。碱性培养基的水解速率高于酸性培养基。结果表明,该药物具有缓释、缓释、延长药物作用和体内性能的特点。
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引用次数: 1
A Rapid and Highly Effectual Protocol for the Synthesis of Bis-coumarins using Triethylaminium-N-sulfonic Acid Tetrachloroaluminate under Solvent-Free Conditions 无溶剂条件下用四氯铝酸三乙胺- n -磺酸快速高效合成双香豆素的方法
IF 5.6 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2019-09-01 DOI: 10.33945/SAMI/CHEMM.2019.5.8
Asieh Kargar-Dolatabadi, A. Zare
In this work, a rapid and highly effectual protocol for the synthesis of       bis-coumarins has been developed. The one-pot quasi three-component reaction of aromatic aldehydes (1 eq.) with 4-hydroxycoumarin (2 eq.) in the presence of catalytic amount of protic acidic ionic liquid triethylaminium-N-sulfonic acid tetrachloroaluminate (TSAT) under solvent-free conditions afforded the mentioned compounds in high yields and short reaction times.
在这项工作中,开发了一种快速高效的双香豆素合成方案。芳香醛(1等)与4-羟基香豆素(2等)在催化量的质子酸离子液体三乙胺- n -磺酸四氯铝酸盐(TSAT)的存在下,在无溶剂条件下进行了一锅准三组分反应,得到了收率高、反应时间短的化合物。
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引用次数: 3
Preparation and Crystal Structure Determination of Zinc (II) Bromide Complexes at the Presence of Various Ligands 不同配体下锌(II)溴化配合物的制备及晶体结构测定
IF 5.6 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2019-09-01 DOI: 10.33945/SAMI/CHEMM.2019.5.2
A. D. Khalaji, E. Shahsavani, M. Dušek, M. Kučeráková, W. Hornfeck
In this paper, we report the syntheses and crystal structuredetermination of three mononuclear and four-coordinated zinc(II) bromide complexes with chemical formula of [Zn(tsc)2]Br2 (1), Zn(PPh3)2Br2 (2) and Zn(Brcatsc)Br2 (3). The synthesized complexes are characterized by elemental analysis (CHN) and theircrystal structures are investigated by single crystal X-ray diffraction. In complex 1, the TSC coordinates to the zinc(II) ion as a bidentate ligand via N and S atoms. In complex 3, the thiosemicarbazone ligand Brcatsc coordinates to zinc(II) ion as a monodentate ligand via S atom. In these complexes, the zinc(II) ion coordinated in a distorted tetrahedral coordination geometry.
本文报道了化学式为[Zn(tsc)2]Br2(1)、Zn(PPh3)2Br2(2)和Zn(Brcatsc)Br2(3)的三种单核四配位溴化锌配合物的合成和晶体结构的测定。用元素分析(CHN)对合成的配合物进行了表征,并用单晶x射线衍射对其晶体结构进行了研究。在配合物1中,TSC通过N和S原子与锌离子作为双齿配体进行配位。在配合物3中,硫代氨基脲配体Brcatsc作为单齿配体通过S原子与锌(II)离子配位。在这些配合物中,锌(II)离子以扭曲的四面体配位几何配位。
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引用次数: 0
The AIM, RDG, NBO, Quantum and Structural Study of Adsorption of Phosgene Gas on the Surface of Pristine and Al, P Doped Ga12N12 Nano Cluster: A DFT Method 光气气体在原始和Al, P掺杂Ga12N12纳米簇表面吸附的AIM, RDG, NBO,量子和结构研究:DFT方法
IF 5.6 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2019-09-01 DOI: 10.33945/SAMI/CHEMM.2019.5.4
P. Hosseini, M. Sameti
The main objective of this work is to study the sensivity of pristine, Al, P and Al & P doped Ga12N12 to adsorb phosgene (COCl2) molecule. The interaction of COCl2 from O, C and Cl sites on the surface of Ga12N12 is investigated by applying the density functional theory (DFT) at the cam-B3LYP/6-31G(d) level of theory.  The geometrical and electrical structures, quantum descriptive, thermodynamic parameters, solvent effect, atom in molecule theory (AIM), natural bond orbital (NBO), and the reduced density gradient (RDG) are calculated at the above level of theory. The calculated results indicate that the adsorption of COCl2 on the surface of pristine and Al, P and Al & P doped Ga12N12 is exothermic, as well as Al-doped Ga12N12 is more favorable than P and Al & P doped. The recovery time results for adsorption of COCl2 from O site on the surface of Ga12N12, Al-Ga11N12, Ga12N11P and Al-Ga11N11P are 0.103, 4.69×10-7, 3.81×10-12 and 4.31×10-7 respectively. As a result, these nanoclusters can be used as sensor devices toward COCl2 molecule. The deformation energy results reveal that the structural change of Ga12N12 and COCl2 at all adsorption states are not significant. The AIM, RDG and NBO results demonstrate that the intermolecular interaction from O site of COCl2 on the surface of pristine, Al, P and Al & P doped Ga12N12 is stronger than C and Cl atoms sites of COCl2 as it is an electrostatic attractive type. The main objective of this work is to study the sensivity of pristine, Al, P and Al & P doped Ga12N12 to adsorb phosgene (COCl2) molecule. The interaction of COCl2 from O, C and Cl sites on the surface of Ga12N12 is investigated by applying the density functional theory (DFT) at the cam-B3LYP/6-31G(d) level of theory.  The geometrical and electrical structures, quantum descriptive, thermodynamic parameters, solvent effect, atom in molecule theory (AIM), natural bond orbital (NBO), and the reduced density gradient (RDG) are calculated at the above level of theory. The calculated results indicate that the adsorption of COCl2 on the surface of pristine and Al, P and Al & P doped Ga12N12 is exothermic, as well as Al-doped Ga12N12 is more favorable than P and Al & P doped. The recovery time results for adsorption of COCl2 from O site on the surface of Ga12N12, Al-Ga11N12, Ga12N11P and Al-Ga11N11P are 0.103, 4.69×10-7, 3.81×10-12 and 4.31×10-7 respectively. As a result, these nanoclusters can be used as sensor devices toward COCl2 molecule.
本研究的主要目的是研究原始的、Al、P和Al & P掺杂的Ga12N12对光气(COCl2)分子的吸附灵敏度。应用密度泛函理论(DFT)在cam-B3LYP/6-31G(d)理论水平上研究了Ga12N12表面O、C和Cl位点上COCl2的相互作用。在以上理论水平上计算了其几何和电学结构、量子描述、热力学参数、溶剂效应、分子原子理论(AIM)、自然键轨道(NBO)和还原密度梯度(RDG)。计算结果表明,COCl2在原始和Al、P、Al & P掺杂Ga12N12表面的吸附是放热的,且Al掺杂Ga12N12比P和Al & P掺杂Ga12N12更有利。Ga12N12、Al-Ga11N12、Ga12N11P和Al-Ga11N11P表面O位COCl2的吸附恢复时间分别为0.103、4.69×10-7、3.81×10-12和4.31×10-7。因此,这些纳米团簇可以作为COCl2分子的传感器器件。变形能结果表明,Ga12N12和COCl2在所有吸附状态下的结构变化都不显著。AIM、RDG和NBO结果表明,原始、Al、P和Al & P掺杂的Ga12N12表面COCl2的O原子位置的分子间相互作用强于COCl2的C和Cl原子位置,因为它是一种静电吸引类型。本研究的主要目的是研究原始的、Al、P和Al & P掺杂的Ga12N12对光气(COCl2)分子的吸附灵敏度。应用密度泛函理论(DFT)在cam-B3LYP/6-31G(d)理论水平上研究了Ga12N12表面O、C和Cl位点上COCl2的相互作用。在以上理论水平上计算了其几何和电学结构、量子描述、热力学参数、溶剂效应、分子原子理论(AIM)、自然键轨道(NBO)和还原密度梯度(RDG)。计算结果表明,COCl2在原始和Al、P、Al & P掺杂Ga12N12表面的吸附是放热的,且Al掺杂Ga12N12比P和Al & P掺杂Ga12N12更有利。Ga12N12、Al-Ga11N12、Ga12N11P和Al-Ga11N11P表面O位COCl2的吸附恢复时间分别为0.103、4.69×10-7、3.81×10-12和4.31×10-7。因此,这些纳米团簇可以作为COCl2分子的传感器器件。
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引用次数: 4
Preparation and Characterization of ZnO Nanoparticles via Thermal Decomposition from Zinc(II) Schiff Base Complex as New Precursor 以锌(II)希夫碱配合物为前驱体热分解法制备ZnO纳米颗粒及表征
IF 5.6 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2019-09-01 DOI: 10.33945/SAMI/CHEMM.2019.5.6
A. D. Khalaji
In this paper,nano-sized of mononuclear tetrahedral zinc(II) complex with the general formula of Zn((pma-ba)2en)Br2.2H2O, (pma-ba)2en=N,N¢-bis{(paramethylamino)benzylidene}ethylenediamine, was synthesized by ultrasonic bath assisted from the reaction of ZnBr2 and Schiff base ligand (pma-ba)2en in molar ratio 1:1 in methanol solution. The zinc(II) Schiff base complex characterized by elemental analyses (CHN), Fourier transformed infra-red (FT-IR) spectroscopy, X-ray powder diffraction (XRD) and scanning electron microscopy (SEM). Also, thermal stability of the complex was studied from room temperature to 780 °C under argon atmosphere. TGA shows three stages for decomposition of the zinc(II) complex. At the end of decomposition, the remainder part is ZnO. The preparation of ZnO at the end of thermal decomposition confirmed with XRD. The XRD pattern of complex has shown that the sharp crystalline peaks indicating the crystalline phase in complex. By Scherrer’s formula, the average size of the nano-sizes of the complex was calculated >200 nm, that confirmed by SEM image. In addition, ZnO nanoparticles were obtained by thermal decomposition of zinc(II) Schiff base complex at 550 °C for 3 h. XRD result that the good crystallinity for zinc(II) oxide with no impurity observed in the ZnO product. The average size of the nanoparticles of the ZnO was calculated <50 nm.
本文以ZnBr2和希夫碱配体(pma-ba)2en为原料,在甲醇溶液中以1:1的摩尔比,利用超声波辅助浴法制备了纳米尺寸的单核四面体锌(II)配合物,其通式为Zn((pma-ba)2en)Br2.2H2O, (pma-ba)2en=N,Nⅱ-二{(参氨基)苄基}乙二胺。采用元素分析(CHN)、傅里叶变换红外光谱(FT-IR)、x射线粉末衍射(XRD)和扫描电子显微镜(SEM)对锌(II)希夫碱配合物进行了表征。同时,研究了该配合物在室温至780℃氩气氛下的热稳定性。热重分析表明锌(II)配合物的分解分为三个阶段。分解结束时,剩余部分为ZnO。用XRD证实了热分解后ZnO的制备。配合物的XRD谱图表明,尖锐的晶峰表明配合物的晶相。根据Scherrer公式,计算出配合物的纳米尺寸的平均尺寸>200 nm,并通过SEM图像证实了这一点。此外,将锌(II)希夫碱配合物在550℃下热分解3 h,得到ZnO纳米颗粒。XRD结果表明,ZnO产品具有良好的结晶度,无杂质。计算得到ZnO纳米颗粒的平均尺寸<50 nm。
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引用次数: 3
Preconcentration of Silver Using Solidification of Floating Organic Drop and Its Determination by Flame Atomic Absorption Spectroscopy 有机悬浮液凝固预富集银及其火焰原子吸收光谱法测定
IF 5.6 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2019-09-01 DOI: 10.33945/SAMI/CHEMM.2019.5.7
H. Noorizadeh, S. Abbasi
A simple, rapid and dispersive liquid–liquid microextraction-solidification of floating organic drop procedure was combined with flame atomic absorption spectrometry and established for the determination of trace amounts of silver. 5-(4-dimethylamino-benzylidine) (Rhodenylene) ligand and 1-dodecanol were used as complexing agents and extracting solvents, respectively. The optimum extraction efficiency of silver was obtained after optimization of the pH, concentration of ligand, the nature and amount of solvent extraction, salt increase effect, extraction time, extraction temperature and stirring rate. The effects of various ions on the recovery of Ag were also investigated. The limit of detection defined as 3SB/m was 1.55 ngL−1. The sensitivity for three eight measurements of 10 and 100 μgL−1 of silver was 1.55 ngL−1. The relative standard deviation (RSD) for the measurements of 0.20 μgL−1 of silver was ±2.3%. Water well, mineral water and urban drinking water samples were analyzed for Ag amount. The microextraction method was satisfactorily used for the determination of Ag in various environmental waters.
建立了一种简便、快速、分散的液液微萃取-凝固有机浮液法与火焰原子吸收光谱法相结合的测定痕量银的方法。以5-(4-二甲氨基苄基)(Rhodenylene)配体和1-十二醇分别作为络合剂和萃取溶剂。通过对pH、配体浓度、溶剂萃取性质及用量、加盐效果、萃取时间、萃取温度、搅拌速率等因素的优化,获得了银的最佳萃取效率。研究了不同离子对银回收的影响。以3SB/m定义的检出限为1.55 ngL−1。测定10 μ l−1和100 μ l−1银的3 ~ 8次灵敏度为1.55 μ l−1。0.20 μgL−1银的相对标准偏差(RSD)为±2.3%。对井水、矿泉水和城市饮用水样品进行了银含量分析。微萃取法可用于各种环境水体中银的测定。
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引用次数: 3
Solvent Free Stereoselective Iodoacetoxylation of Alkenes and Glycals Using N-Iodosuccinimide and Acetic Anhydride 用n -碘丁二酰亚胺和乙酸酐进行无溶剂立体选择性烯烃和甘油的碘乙酰氧基化
IF 5.6 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2019-09-01 DOI: 10.33945/SAMI/CHEMM.2019.5.9
A. R. Reddy, S. Farooq, B. Dar
The reactions of glycals with N-iodosuccinimide and acetic anhydride under solvent free conditions provide 2-deoxy-2-iodo-α-mannopyranosyl acetates with good stereoselectivity. The developed process is in accordance with principles of green chemistry and addresses the shortage of such methods for the regioselective iodo acetoxylation of alkenes.
甘醛与n -碘丁二酰亚胺和乙酸酐在无溶剂条件下反应得到立体选择性好的2-脱氧-2-碘-α-甘露吡喃酰乙酸酯。该工艺符合绿色化学原理,解决了烯烃区域选择性碘乙酰氧基化方法的不足。
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引用次数: 0
Effects of Freeze-drying and Freezing on Vitamins and Sugars of Mango Pulp (‘Apple’ Cultivar): A Preliminary Comparison of Methods for Improving Sample Storage 冻干和冷冻对芒果果肉(‘苹果’品种)维生素和糖的影响:改善样品保存方法的初步比较
IF 5.6 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2019-08-20 DOI: 10.33945/sami/chemm.2019.6.10
K. Olale, W. Waudo, S. A. Mohammed
Mango (Mangifera indica L.) fruits are highly perishable ones whose important nutrients such as vitamins and sugars quickly decrease under storage. In this study, we compared two methods of fruit pulp storage; freezing and freeze-drying in order to compare total carotenoids, β-carotene, ascorbic acid (AA), titratable acidity (TTA), total soluble solid (TSS) and pH. Mean total carotenoid, β-carotene and AA of frozen pulp were 7.08±0.15 µg/g, 1.47±0.09 µg/g and 92.77±17.49 mg/100 g respectively. While freeze-dried pulp had 8.06±0.03 µg/g, 2.35±0.03 µg/g and 113.02±0.07 mg/100 g for total carotenoid, β-carotene and AA respectively. The total carotenoid, β-carotene and AA of fresh pulp were; 8.15 µg/g, 2.44 µg/g and 119 mg/100 g respectively. TTA, TSS and pH were; 3.01±1.01%, 9.40±1.42 °Brix and 2.97±0.19 for frozen pulp and 2.97±0.01%, 11.70±0.08 °Brix and 2.99±0.01 for freeze dried pulp respectively. TTA, TSS and pH for fresh pulp were; 4.85%, 11.90 Brix% and 3.48 respectively. All measured parameters were significantly higher (P<0.05) in fresh sample than in the stored pulp (frozen or freeze-dried). Mean total carotenoids, β carotene, AA and TSS were significantly (p<0.05) higher for freeze-dried pulp than for frozen pulp. However, mean TTA and pH did not differ between freeze-dried and frozen pulp. Slow decrease of AA in the freeze-dried pulp further suggests the method as preferred for long term storage of mango pulps.
芒果(Mangifera indica L.)是极易腐烂的水果,其重要的营养成分如维生素和糖在储存过程中迅速减少。在本研究中,我们比较了两种果肉储存方法;冷冻和冷冻干燥后,果肉的总类胡萝卜素、β-胡萝卜素、抗坏血酸(AA)、可滴定酸度(TTA)、总可溶性固形物(TSS)和ph值的平均值分别为7.08±0.15µg/g、1.47±0.09µg/g和92.77±17.49 mg/100 g。冻干果肉中总类胡萝卜素、β-胡萝卜素和AA含量分别为8.06±0.03µg/g、2.35±0.03µg/g和113.02±0.07 mg/100 g。鲜果肉的总类胡萝卜素、β-胡萝卜素和AA含量分别为;分别为8.15µg/g、2.44µg/g和119 mg/100 g。TTA、TSS、pH分别为;冷冻纸浆Brix分别为3.01±1.01%、9.40±1.42°和2.97±0.19;冻干纸浆Brix分别为2.97±0.01%、11.70±0.08°和2.99±0.01。新鲜果肉的TTA、TSS和pH分别为;Brix%分别为4.85%、11.90和3.48。新鲜纸浆的各项测定指标均显著高于贮藏纸浆(冷冻或冻干)。冻干果肉的平均总类胡萝卜素、β胡萝卜素、AA和TSS显著高于冷冻果肉(p<0.05)。冻干浆和冷冻浆的平均TTA和pH值无显著差异。冻干果肉中AA的缓慢下降进一步表明该方法是长期储存芒果果肉的首选方法。
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引用次数: 0
期刊
Chemical Methodologies
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