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Development of a method for the detection of amixin and amizon by HPLC on SunFire C18 column SunFire C18色谱柱高效液相色谱法测定氨虫素和氨虫素的方法
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-08-07 DOI: 10.6001/chemija.v33i3.4750
Anastasiia Belikova, Anna Materienko, Ludmila Sidorenko, Olha Chorna, Deividas Burdulis, V. Georgiyants
A method for the determination of amizone and amixin in the same sample and in their mixture with antibiotics (ceftriaxone, tetracycline, ampicillin and levofloxacin) was developed using reversed-phase highperformance liquid chromatography equipped with a photodiode array detector. A SunFire C18 column, a mobile phase consisting of sodium perchlorate buffer (pH = 2.5) and acetonitrile (75:25), at a flow rate of 0.8 ml/min, was used. The analytes were identified at 205 and 265 nm. The specificity, linearity, precision parameters, LOD and LOQ were evaluated during the validation of the methodology, and the correlation coefficients of amizone and amixin were 0.9992 and 0.9998, respectively. This method can also be used for the determination of amizone and amixin and their presence in a mixture with antibiotics in the environment.
建立了用光电二极管阵列检测器反相高效液相色谱法测定同一样品中阿米松和阿米辛及其与抗生素(头孢曲松、四环素、氨苄西林和左氧氟沙星)混合物中阿米松和阿米辛的含量。采用SunFire C18色谱柱,流动相为高氯酸钠缓冲液(pH = 2.5)和乙腈(75:25),流速为0.8 ml/min。分析物在205和265 nm处鉴定。方法验证时进行了特异性、线性度、精密度参数、定量限和定量限评价,结果表明:阿米唑酮和阿米辛的相关系数分别为0.9992和0.9998。本方法也可用于测定环境中抗生素混合物中阿米松和阿米辛的含量。
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引用次数: 0
Determination of pyridine and furfuryl alcohol in breath after coffee consumption 饮用咖啡后呼出气体中吡啶和糠醇的测定
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-08-07 DOI: 10.6001/chemija.v33i3.4751
Adrián Vicent Claramunt, Audrius Sadaunykas, Birutė Knašienė, E. Naujalis
We aimed to demonstrate that breath analysis can be used as a method for the detection of potentially harmful compounds in food after their ingestion. Development of such a method could be adapted as a tool for detection of food intoxication. To achieve this, we compared the levels of pyridine (Py) and furfuryl alcohol (FFA) found in breath with the quantity of these compounds ingested when drinking coffee. Coffee drink beverages were prepared in the laboratory and consumed by volunteers (n = 5). An aliquot of coffee was analysed using high performance liquid chromatography with diode-array detection (HPLC-DAD) to quantify Py and FFA in the beverage. Breath samples were collected several times over a 45 min period after ingestion of coffee and analysed by thermal desorption coupled to gas chromatography/mass spectrometry (TD/GC-MS). The levels of Py and FFA found in coffee ranged from 0.2 to 3 mg/cup of coffee, and from 7 to 30 mg/cup of coffee, respectively. The levels of these compounds detected in breath ranged from 7 to 1200 ng/l breath for Py and from 1 to 760 ng/l breath for FFA. Several parameters can influence the levels of these chemicals in breath, especially the collection time of the breath sample.
我们的目的是证明呼气分析可以作为一种检测食物摄入后潜在有害化合物的方法。这种方法的发展可以作为一种检测食物中毒的工具。为了实现这一目标,我们将呼吸中发现的吡啶(Py)和糠醇(FFA)的含量与饮用咖啡时摄入的这些化合物的含量进行了比较。在实验室中制备咖啡饮料,并由志愿者饮用(n = 5)。使用高效液相色谱二极管阵列检测(HPLC-DAD)对咖啡进行分析,以定量饮料中的Py和FFA。在摄入咖啡后45分钟内多次收集呼气样本,并通过热解吸和气相色谱/质谱(TD/GC-MS)分析。在咖啡中发现的Py和FFA含量分别在0.2到3毫克/杯和7到30毫克/杯之间。在呼吸中检测到的这些化合物的水平,Py为7至1200 ng/l, FFA为1至760 ng/l。有几个参数可以影响呼吸中这些化学物质的水平,特别是呼吸样本的收集时间。
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引用次数: 1
Corrosion resistance of AZ31 alloy after treatment with high current density impulse or/and laser irradiation in Hank’s solution AZ31合金在Hank’s溶液中高电流密度脉冲或/和激光辐照后的耐蚀性
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-08-07 DOI: 10.6001/chemija.v33i3.4748
G. Bikulčius, S. Lichušina, V. Pakštas, M. Gedvilas, V. Stankevič, A. Selskienė, A. Grigucevičienė
In this article, we have introduced a new method that can improve the corrosion resistance of AZ31 alloy. We compared the biodegradation of AZ31 alloy foil treated with a high current density impulse (HCDI), laser irradiation (LI) and HCDI-LI with that of the untreated one. The rate of the biodegradation of AZ31 alloy treated with HCDI-LI was lower than those of the untreated one, the alloy treated with HCDI or LI. Thus, the improved corrosion resistance of the AZ31 alloy treated with HCDI-LI allows its use for medical purposes.
本文介绍了一种提高AZ31合金耐蚀性的新方法。比较了高电流密度脉冲(HCDI)、激光照射(LI)和HCDI-LI处理的AZ31合金箔与未处理AZ31合金箔的生物降解情况。AZ31合金经HCDI-LI处理后的生物降解率低于未处理AZ31合金、HCDI和LI处理的AZ31合金。因此,经HCDI-LI处理的AZ31合金的耐腐蚀性得到改善,可用于医疗目的。
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引用次数: 0
The validated method for the analysis of a mixture of psychotropic medicines olanzapine, clorazepate and escitalopram using a high-performance liquid chromatography method 建立了一种高效液相色谱法分析精神药物奥氮平、氯硝西酯和艾司西酞普兰混合物的方法
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-05-04 DOI: 10.6001/chemija.v33i2.4706
Mamdouh Alasabashi, A. Ževžikovienė, M. Marksa, Laura Rimkiene, A. Ževžikovas
It was established that self-poisoning with antipsychotics, anti-anxiety drugs and antidepressants is caused by consumption of the drug in higher doses than prescribed. So it is very important to determine fast the materials causing poisoning and use the method which would allow one to identify several substances during only one analysis. Reference and test solutions were prepared in ethanol. A qualitative and quantitative analysis was carried out on a Waters Alliance 2695 liquid chromatograph equipped with a Waters 996 PDA detector and an ACE C18 (250 mm × 4.6 mm × 5 μm) column. The mobile phase consisted of solvent trifluoroacetic acid (0.1 %) and acetonitrile. The linear gradient elution profile was used. For the validation process the following parameters were chosen: specificity, repeatability, precision and limits (LOD and LOQ). According to the study results, it can be concluded that the validated method for the qualitative and quantitative evaluation analysis of olanzapine, clorazepate and escitalopram was developed.
已经确定的是,服用抗精神病药物、抗焦虑药物和抗抑郁药物的自我中毒是由于服用剂量高于处方剂量造成的。因此,快速确定引起中毒的物质和使用在一次分析中可以识别多种物质的方法是非常重要的。在乙醇中制备参比液和被试液。采用Waters Alliance 2695型液相色谱仪,配备Waters 996 PDA检测器和ACE C18 (250 mm × 4.6 mm × 5 μm)色谱柱进行定性和定量分析。流动相为溶剂三氟乙酸(0.1%)和乙腈。采用线性梯度洗脱剖面。对于验证过程,选择以下参数:特异性、重复性、精密度和限(LOD和LOQ)。根据研究结果,建立了奥氮平、氯硝西酯和艾司西酞普兰的定性和定量评价分析方法。
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引用次数: 0
Synthesis of pyrimidines containing hydroxamic acid, 1,3,4-oxadiazole or 1,2,4-triazole moieties as potential HDAC inhibitors 合成含有羟基肟酸、1,3,4-恶二唑或1,2,4-三唑的嘧啶类潜在HDAC抑制剂
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-05-04 DOI: 10.6001/chemija.v33i2.4708
V. Jakubkienė, Mantas Žvirblis, S. Tumkevičius
The histone deacetylases (HDACs) play an essential role in the transcriptional regulation of cells through deacetylation of nuclear histone proteins and are promising therapeutic targets for treatment of various diseases. Therefore, interest to the design and synthesis of novel HDAC inhibitors, among which hydroxamic acids occupy an important place, has been constantly increasing in recent years. Here, synthesis of pyrimidines with 1,3,4-oxadiazole or 1,2,4-triazole and hydroxamic acid moieties as potential HDAC inhibitors is described. The target compounds were obtained by sequential reactions of (O- and N-pyrimidinyl)alkanoates with hydrazine hydrate followed by cyclization reaction of the obtained hydrazides with potassium O-ethyl xanthate and alkylation of the synthesised oxadiazole(triazole)thiones with 2-chloro-N-hydroxyacetamide. One of 1,3,4-oxadiazole-2-thiones under the treatment with hydrazine hydrate underwent the recyclisation reaction to give the corresponding 4-amino-1,2,4-triazole. Investigation of the inhibitory activity of the synthesised compounds against HDAC4 and HDAC8 isoforms revealed that N-hydroxy-2-(5-(4-(6-(6-methyl-2-(methylthio)pyrimidin-4-yloxy) butyl)-1,3,4-oxadiazol-2-ylthio)acetamide exhibited a weak inhibitory activity against HDAC8 isoform (IC50 = 12.7 μM).
组蛋白脱乙酰酶(HDAC)通过核组蛋白的脱乙酰作用在细胞的转录调控中发挥着重要作用,是治疗各种疾病的有前景的治疗靶点。因此,近年来,人们对新型HDAC抑制剂的设计和合成越来越感兴趣,其中异羟肟酸占有重要地位。本文描述了用1,3,4-恶二唑或1,2,4-三唑和异羟肟酸部分合成嘧啶作为潜在的HDAC抑制剂。目标化合物是通过(O-和N-嘧啶基)烷酸酯与肼水合物的顺序反应,然后所获得的肼与O-乙基黄原酸钾的环化反应,以及合成的恶二唑(三唑)硫酮与2-氯-N-羟基乙酰胺的烷基化反应而获得的。1,3,4-恶二唑-2-硫酮中的一种在水合肼处理下进行循环反应,得到相应的4-氨基-1,2,4-三唑。对合成的化合物对HDAC4和HDAC8异构体的抑制活性的研究表明,N-羟基-2-(5-(4-(6-(6-甲基-2-(甲硫基)嘧啶-4-基氧基)丁基)-1,3,4-恶二唑-2-硫基)乙酰胺对HDAC8亚型表现出弱的抑制活性(IC50=12.7μM)。
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引用次数: 0
The comparative study of redox properties of recombinant human cytosolic and mitochondrial NADPH: thioredoxin reductases 重组人细胞质和线粒体NADPH:硫氧还蛋白还原酶氧化还原特性的比较研究
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-05-04 DOI: 10.6001/chemija.v33i2.4707
Lina Misevičienė, K. Krikštopaitis, N. Čėnas
We compared the redox properties of recombinant cytosolic (TrxR1) and mitochondrial (TrxR2) isoforms of human flavosulfoselenoenzyme NADPH:thioredoxin reductase. The standard redox potentials of isoenzymes (E0 7), determined according to the redox equilibrium with the NADP+/NADPH couple, were equal to –0.295 V (TrxR1) and –0.270 V (TrxR2). The more positive value of E0 7 of TrxR2 may be attributed to the presence of His-125 at the vicinity of catalytic disulfide and selenylsulfide, instead of Tyr-116 in TrxR1. The reactivity of several quinones and nitroaromatic compounds towards TrxR1 and TrxR2 increased with their single-electron reduction potential (E1 7). For the first time, we studied the TrxR1-catalysed reduction of a series of aromatic N-oxides which were reduced in a mixed single- and two-electron way. Their reactivity was close to that of quinones and nitroaromatics with the similar values of E1 7.
我们比较了重组人黄磺基硒酶NADPH:硫氧还蛋白还原酶的细胞质(TrxR1)和线粒体(TrxR2)异构体的氧化还原特性。根据NADP+/NADPH对氧化还原平衡测定的同工酶(e07)的标准氧化还原电位分别为-0.295 V (TrxR1)和-0.270 V (TrxR2)。TrxR2的e07较高的正值可能是由于His-125存在于催化二硫化物和硒基硫化物附近,而不是TrxR1中的tyrl -116。几种醌类和硝基芳香化合物对TrxR1和TrxR2的反应活性随着其单电子还原电位的增加而增加(E1 7)。我们首次研究了TrxR1催化的一系列芳香n -氧化物的单电子和双电子混合还原。它们的反应活性接近醌类和硝基芳烃类,E1 - 7值相近。
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引用次数: 0
Curing of epoxy resins by bio-based phenalkamines vs low-molecular-weight amines: study by DSC 生物基苯烷胺与低分子量胺固化环氧树脂的DSC研究
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-05-04 DOI: 10.6001/chemija.v33i2.4709
J. Jonikaitė-Švėgždienė, Liepa Pastarnokienė, Virginija Juknevičiūtė, R. Makuška
In this study, curing of BPA-based epoxy resins Araldite®GY-2600 and Araldite®GY-240 by low-molecular-weight amines EDA, TETA and Jeffamine D-230, and bio-based phenalkamines Cardolite®NX-6019, Cardolite®Lite-2002 and Cardolite®GX-6004 was studied by differential scanning calorimetry (DSC) and rheology measurements. DSC provided quantitative information on the overall reaction kinetics (the enthalpy of curing reaction, ΔHR; cure degree, α; curing reaction rate, dα/dt) and the glass transition temperature (Tg) of the cured product. It was demonstrated that the DSC curing of epoxy resins by phenalkamines started at lower temperature, and the curing rates were slightly lower compared to those cured by low-molecular-weight amine hardeners. The enthalpy of the curing by phenalkamines was lower, especially in the case of more viscous epoxy resin GY-2600. Tg of the cured epoxy resins varied from 50 to 98°C and was slightly lower when cured with cardanol-based phenalkamines. The results demonstrate that curing of epoxy resins by bio-based phenalkamines proceeds in a similar temperature interval like using low-molecular-weight amines as hardeners but with less exothermic effect, which could be an advantage.
在本研究中,通过差示扫描量热法(DSC)和流变学测量研究了低分子量胺EDA、TETA和Jeffamine D-230以及生物基苯烷胺Cardolite®NX-6019、Cardolite™Lite-2002和Cardolite?GX-6004对BPA基环氧树脂Araldite®GY-2600和Araldite™GY-240的固化。DSC提供了关于整个反应动力学(固化反应焓ΔHR;固化度α;固化反应速率dα/dt)和固化产物的玻璃化转变温度(Tg)的定量信息。结果表明,苯烷胺对环氧树脂的DSC固化在较低的温度下开始,与低分子量胺固化剂相比,固化速率略低。酚烷胺的固化焓较低,尤其是在粘度较大的环氧树脂GY-2600的情况下。固化的环氧树脂的Tg在50至98°C之间变化,当用腰果醇基酚烷胺固化时,Tg略低。结果表明,生物基苯烷胺对环氧树脂的固化在类似的温度区间内进行,就像使用低分子量胺作为固化剂一样,但放热效应较小,这可能是一个优势。
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引用次数: 4
A novel method for the formation of bioceramic nano-calcium hydroxyapatite coatings using sol-gel and dissolution-precipitation processing 溶胶-凝胶-溶解沉淀法制备生物陶瓷纳米钙羟基磷灰石涂层的新方法
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-05-04 DOI: 10.6001/chemija.v33i2.4705
Rasa Karalkevičienė, Greta Briedytė, T. Murauskas, Mantas Norkus, A. Zarkov, J. Yang, A. Kareiva
The wet chemistry route has been developed to prepare calcium hydroxyapatite (Ca10(PO4)6(OH)2, (HA)) thin films on a silicon substrate using the novel low-temperature sol-gel and dissolution-precipitation approach. The calcium carbonate thin films on the silicon substrate were obtained by spin-coating technique when substrates were repeatedly coated with 10, 20 and 30 layers of sol-gel solution. The composites formed of crystalline and amorphous CaCO3 were obtained by calcination of the coatings for different time at 600°C. A dissolution-precipitation procedure was used for the preparation of calcium hydroxyapatite thin films on silicon substrate at 80°C. The obtained synthesis products were characterised by X-ray powder diffraction (XRD) analysis, scanning electron microscopy (SEM) and Raman spectroscopy.
采用新型低温溶胶-凝胶-溶解-沉淀法,在硅衬底上制备了钙羟基磷灰石(Ca10(PO4)6(OH)2,(HA))薄膜。通过旋涂技术,在硅衬底上反复涂10层、20层和30层溶胶-凝胶溶液,获得了碳酸钙薄膜。通过在600°C下煅烧不同时间的涂层,获得了由结晶和无定形CaCO3形成的复合材料。采用溶解沉淀法在80°C下在硅衬底上制备羟基磷灰石钙薄膜。通过X射线粉末衍射(XRD)分析、扫描电子显微镜(SEM)和拉曼光谱对所获得的合成产物进行了表征。
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引用次数: 0
Profiling of volatile organic compounds for environment discrimination in Vilnius City 维尔纽斯市用于环境识别的挥发性有机化合物图谱
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-02-07 DOI: 10.6001/chemija.v33i1.4661
A. V. Claramunt, Audrius Sadaunykas, Simonas Balčiūnas, Birutė Knašienė, Audrius Zolumskis, E. Naujalis
The aim of this study was to show how volatile organic compounds (VOCs) profiling can be used as a method to identify different environments across a city. To achieve that, we employed several methods. First, we carried out the profiling of VOCs in several different locations. Then we identified the marker compounds and their sources. Air samples were collected from 6 different locations within the Vilnius City centre using thermal desorption (TD) tubes. Samples were analysed using thermal desorption coupled with gas chromatography mass spectroscopy (TD/GC-MS) methodology. Compound identification was performed by the library match using the NIST MS Search 2.0 (2005) mass spectral library. The results show how variation in the levels of different VOCs can distinguish between locations within a relatively small area of 2 km2 depending on different emission sources.
这项研究的目的是展示挥发性有机化合物(VOCs)分析如何被用作识别城市不同环境的方法。为了达到这个目的,我们采用了几种方法。首先,我们对几个不同地点的VOCs进行了分析。然后我们确定了标记化合物及其来源。使用热解吸(TD)管从维尔纽斯市中心的6个不同地点收集空气样本。采用热解吸-气相色谱-质谱联用(TD/GC-MS)方法对样品进行分析。化合物鉴定采用NIST MS Search 2.0(2005)质谱库匹配。结果表明,不同挥发性有机化合物水平的变化如何根据不同的排放源在相对较小的2平方公里范围内区分不同地点。
{"title":"Profiling of volatile organic compounds for environment discrimination in Vilnius City","authors":"A. V. Claramunt, Audrius Sadaunykas, Simonas Balčiūnas, Birutė Knašienė, Audrius Zolumskis, E. Naujalis","doi":"10.6001/chemija.v33i1.4661","DOIUrl":"https://doi.org/10.6001/chemija.v33i1.4661","url":null,"abstract":"The aim of this study was to show how volatile organic compounds (VOCs) profiling can be used as a method to identify different environments across a city. To achieve that, we employed several methods. First, we carried out the profiling of VOCs in several different locations. Then we identified the marker compounds and their sources. Air samples were collected from 6 different locations within the Vilnius City centre using thermal desorption (TD) tubes. Samples were analysed using thermal desorption coupled with gas chromatography mass spectroscopy (TD/GC-MS) methodology. Compound identification was performed by the library match using the NIST MS Search 2.0 (2005) mass spectral library. The results show how variation in the levels of different VOCs can distinguish between locations within a relatively small area of 2 km2 depending on different emission sources.","PeriodicalId":9720,"journal":{"name":"Chemija","volume":" ","pages":""},"PeriodicalIF":0.6,"publicationDate":"2022-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46211880","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Microwave synthesis of silver core-silica decorated nanoparticles 微波合成银芯-二氧化硅修饰纳米粒子
IF 0.6 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2022-02-07 DOI: 10.6001/chemija.v33i1.4657
Edita Daublytė, Agnė Zdaniauskienė, T. Charkova
The silver nanospheres (70 ± 5 nm) were synthesised and decorated with silica under microwave irradiation. The obtained silver core-silica decorated nanoparticles (80 ± 5 nm) were applied for 4-mercaptobenzoic acid monolayer analysis by shell-isolated nanoparticle-enhanced Raman spectroscopy. A detailed protocol of synthesis, characterisation by UV/Vis, HR-TEM and Raman techniques are represented here.
合成了银纳米球(70±5nm),并在微波辐射下用二氧化硅进行了修饰。通过壳分离的纳米颗粒增强拉曼光谱,将获得的银核二氧化硅修饰的纳米颗粒(80±5nm)应用于4-巯基苯甲酸单层分析。本文介绍了合成、UV/Vis、HR-TEM和拉曼技术表征的详细方案。
{"title":"Microwave synthesis of silver core-silica decorated nanoparticles","authors":"Edita Daublytė, Agnė Zdaniauskienė, T. Charkova","doi":"10.6001/chemija.v33i1.4657","DOIUrl":"https://doi.org/10.6001/chemija.v33i1.4657","url":null,"abstract":"The silver nanospheres (70 ± 5 nm) were synthesised and decorated with silica under microwave irradiation. The obtained silver core-silica decorated nanoparticles (80 ± 5 nm) were applied for 4-mercaptobenzoic acid monolayer analysis by shell-isolated nanoparticle-enhanced Raman spectroscopy. A detailed protocol of synthesis, characterisation by UV/Vis, HR-TEM and Raman techniques are represented here.","PeriodicalId":9720,"journal":{"name":"Chemija","volume":" ","pages":""},"PeriodicalIF":0.6,"publicationDate":"2022-02-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47139767","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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