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Development and Validation of an RP-HPLC Method for the Quantitative Analysis of Triclosan in Human Urine 人尿中三氯生反相高效液相色谱定量分析方法的建立与验证
4区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-11-13 DOI: 10.1155/2023/6684834
Prince Karikari, James Oppong-Kyekyeku, Edmund Ekuadzi, Samuel Oppong Bekoe, Rita Opoku, Daniel Nimako Amprako, Emmanuel Addo-Yobo, Sandra Kwarteng Owusu, Bernard Arhin, Adegoke G. Falade, Ganiyu Arinola, Adeleye S. Bakarey, John I. Anetor, Kevin J. Mortimer
Triclosan (TCS), a synthesized chlorinated phenolic compound, is commonly utilized in consumable products as an antimicrobial agent. TCS has sparked widespread awareness because of its toxicity and possible negative effect on public health in recent years. In this study, a highly sensitive, fast, and cost-effective isocratic reversed-phase high-performance liquid chromatography (RP-HPLC) method coupled with solid-phase extraction for analysis of triclosan in human urine samples was developed. The method utilized methanol and water in a ratio of 90 : 10 as the mobile phase on a Phenomenex Luna 3 µm C18(2) 100 Å, 150 × 4.60 mm stationary phase, with a runtime of 5 minutes. The method showed good resolution of triclosan in the presence of the sample matrix. Validation of the method was performed according to the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH). Linearity was tested over a range of 0.00625 µg/mL to 6.4 µg/mL, as accuracy recorded a recovery of 89.25%, 91.0%, and 92.75%. Limits of detection (LOD) and quantification (LOQ) were obtained to be 0.0173 µg/mL and 0.0525 µg/mL, respectively. The method proved to be robust over a temperature range of 26°C, 30°C, and 35°C and a flow rate of 0.5 ml, 1.0 ml, and 1.5 ml. The developed method was employed to detect and quantify triclosan in 153 urine samples, comprising 60 samples from Ibadan, Nigeria, and 93 samples from Kumasi, Ghana. Triclosan was detected in a total of 52 samples with an average content of 0.054588 µg/ml. This method can therefore be used for the routine analysis of triclosan in urine samples.
三氯生(TCS)是一种合成的氯化酚类化合物,通常用作消费品中的抗菌剂。近年来,TCS因其毒性和可能对公众健康产生的负面影响而引起了广泛的关注。本研究建立了一种高灵敏、快速、高性价比的等容反相高效液相色谱(RP-HPLC) -固相萃取法分析人尿样品中三氯生的方法。该方法以甲醇和水的比例为90:10作为流动相,在Phenomenex Luna 3µm C18(2) 100 Å上,固定相为150 × 4.60 mm,运行时间为5分钟。在样品基质存在的情况下,该方法对三氯生具有良好的分辨能力。根据国际人用药品技术要求统一委员会(ICH)对该方法进行验证。在0.00625µg/mL ~ 6.4µg/mL范围内线性关系良好,回收率分别为89.25%、91.0%和92.75%。检出限和定量限分别为0.0173µg/mL和0.0525µg/mL。该方法在26°C、30°C和35°C的温度范围内,以及0.5 ml、1.0 ml和1.5 ml的流速范围内均被证明是可靠的。该方法用于检测和定量153份尿液样本中的三氯生,其中60份来自尼日利亚伊巴丹,93份来自加纳库马西。52份样品中检出三氯生,平均含量为0.054588µg/ml。本方法可用于尿液样本中三氯生的常规分析。
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引用次数: 0
Prediction of Refractive Indices of Binary Mixtures of Ionic Liquids and Water 离子液体与水二元混合物折射率的预测
4区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-11-07 DOI: 10.1155/2023/9934356
Mohd Sajid Ali, Mohammad Tariq
In the present work, we have successfully predicted the refractive indices of binary mixtures containing ionic liquids (ILs) and water as a component following the approach of Gladstone–Dale and Newton. These approaches were proposed as adequate to predict the refractive indices of mixtures containing imidazolium-based ILs with water or ethanol. It requires just the knowledge of the density and refractive index of pure components to obtain the value of refractive index of binary mixtures at any composition. We have selected 30 binary systems that contain ILs from imidazolium, ammonium, pyrrolidinium, and pyridinium families for validation. The tested data comprise of more than 400 mixture points. The results are presented in terms of average percentage deviations (APDs) from the experimental values. The Gladstone–Dale method gives better results compared to the Newton approach. The reasons why these approaches give large APDs for some mixtures are discussed in the manuscript.
本文采用牛顿和格莱斯顿的方法,成功地预测了以水为组分的离子液体二元混合物的折射率。这些方法被认为足以预测含有咪唑基il与水或乙醇的混合物的折射率。只需要知道纯组分的密度和折射率,就可以得到二元混合物在任何组成下的折射率值。我们选择了30个包含咪唑、铵、吡咯吡啶和吡啶家族il的二元体系进行验证。测试数据由400多个混合点组成。结果以与实验值的平均百分比偏差(APDs)表示。与牛顿法相比,格莱斯顿-戴尔法给出了更好的结果。本文讨论了这些方法对某些混合物给出大apd的原因。
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引用次数: 0
Efficient Electro-Oxidation of 2-Propanol at Platinum- and Gold-Modified Palladium Nanocatalysts 2-丙醇在铂和金改性钯纳米催化剂上的高效电氧化
4区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-11-03 DOI: 10.1155/2023/6674344
Kareem Ayman, Yaser M. Asal, Ahmad M. Mohammad, Islam M. Al-Akraa
This study aims at investigating the catalytic performance of Pd, Pd/Pt, and Pd/Au nanocatalysts toward the 2-propanol electro-oxidation reaction (2POR) in an alkaline medium. The catalyst components (Pd, Pt, and Au) were sequentially electrodeposited onto the glassy carbon (GC) electrode surface and further characterized using electrochemical (cyclic voltammetry (CV)) and materials (field-emission scanning electron microscopy (FE-SEM) coupled with energy-dispersive X-ray (EDX)) characterization methods. The Pd/Au/GC catalyst showed the highest catalytic activity in terms of the highest oxidation current (0.386 mA) and the highest stability in terms of the highest obtained current after 1800 s of continuous electrolysis. This behaviour was attributed to the enhancement in the charge transfer kinetics where the Pd/Au/GC catalysts acquired the lowest charge transfer resistance (Rct, 1.85 kΩ) during the 2POR.
研究了Pd、Pd/Pt和Pd/Au纳米催化剂在碱性介质中对2-丙醇电氧化反应(2POR)的催化性能。催化剂组分(Pd, Pt和Au)依次电沉积在玻碳(GC)电极表面,并通过电化学(循环伏安法(CV))和材料(场发射扫描电镜(FE-SEM)耦合能量色散x射线(EDX))表征方法进一步表征。Pd/Au/GC催化剂在连续电解1800 s后的最高氧化电流(0.386 mA)表现出最高的催化活性和最高获得电流的稳定性。这种行为归因于电荷转移动力学的增强,其中Pd/Au/GC催化剂在2POR期间获得了最低的电荷转移阻力(Rct, 1.85 kΩ)。
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引用次数: 0
Copper- and Ligand-Free Sonogashira Cross-Coupling: Access to Novel 3-Aminoindole Derivatives and Their Biological Evaluations 无铜和配体的Sonogashira交叉偶联:新型3-氨基吲哚衍生物的获取及其生物学评价
4区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-11-03 DOI: 10.1155/2023/6668609
Tshikani D. Rikhotso, Kgomotso W. Poopedi, Winston Nxumalo, Tlabo C. Leboho
Indole-containing compounds are widely distributed in the plant and animal kingdom, and their biological activity and pharmacological properties have prompted research into their chemical properties. This study developed a one-pot methodology for the synthesis of 3-aminoindole derivatives using copper- and ligand-free Sonogashira cross-coupling reaction conditions. The synthesised 3-aminoindole derivatives were confirmed using spectroscopic techniques. The resulting 3-aminoindole derivatives were biologically evaluated against Mycobacterium tuberculosis and Plasmodium falciparum. For example, indole derivatives 10a (7.813 µM) and 10j (8.332 µM) were the most active derivatives in the CAS and ADC media, respectively.
含吲哚类化合物广泛存在于动植物界,其生物活性和药理性质促使人们对其化学性质进行研究。本研究在无铜和无配体的Sonogashira交叉偶联反应条件下,建立了一锅法合成3-氨基吲哚衍生物。利用光谱技术对合成的3-氨基吲哚衍生物进行了确证。得到的3-氨基吲哚衍生物对结核分枝杆菌和恶性疟原虫进行了生物学评价。例如,吲哚衍生物10a(7.813µM)和10j(8.332µM)分别是CAS和ADC培养基中最活跃的衍生物。
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引用次数: 0
Antimicrobial Activities of Some Constituents Isolated from a Kenyan Medicinal Plant, Capparis fascicularis DC 肯尼亚药用植物刺槐部分成分的抗菌活性研究
4区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-10-31 DOI: 10.1155/2023/6114501
Mary W. Kagika, Sumesh C. Chhabra, James O. M. Nonoh, Ahmed Hassanali
Background of the Study. Capparis fascicularis DC. is an indigenous medicinal plant belonging to the family Capparaceae found in Nyandarua County, Nairobi, Kenya, and many parts of Africa. It is a shrub whose roots are used traditionally to treat colds. Aim. The aim of the present study is to carry out antimicrobial activities of solvent extracts of different parts of Capparis fascicularis, characterize the phytochemical constituents of the most active extract, and identify the most active compounds. Place and Duration of the Study. All the experiments were carried out in the departments of Chemistry and Microbiology, Kenyatta University, Nairobi, Kenya. Methodology. Petroleum ether, ethyl acetate, methanol, and water extracts from the leaves, stem bark, and root bark of C. fascicularis were screened against selected strains of both Gram-positive (Staphylococcus aureus and Bacillus subtilis) and Gram-negative (Salmonella typhimurium and Escherichia coli) bacteria using disc diffusion and tube dilution methods. Fractionation of the most active crude extract was carried out by column chromatography, and the fractions together with the most active crude extract were screened against the selected bacterial strains. The most active fraction was further fractionated, and the subfractions were screened against the bacterial strains to test for possible synergistic effects between the subfractions and their constituents. The most active fraction was then analysed by GC-MS and LC-ESI-MS methods to identify the major constituents. Results. The ethyl acetate extract of C. fascicularis root bark (CFR2) showed a significant in vitro antibacterial activity. From the seven fractions of CFR2 obtained, fraction 2 (F2) had the lowest MIC value and was thus most active. Moreover, F2 was found to be more active compared to the four subfractions obtained from it. This suggested that constituents of F2 worked in synergy. Fraction 2 contained phenols, terpenes, and flavonoids. Two compounds were identified by GC-MS as 2,4-di-tert-butylphenol and (E,E)-2,4-decadienal, while three compounds were identified by LC-ESI-MS as tanshinone II A, cryptotanshinone, and danshensu. Conclusion. The study revealed that CFR2 is the most active extract on bacteria, suggesting that most antimicrobial compounds are concentrated in the roots of C. fascicularis. A follow-up study is directed towards chromatographic separations to obtain the other chemical constituents and screen them against various strains of bacteria.
研究背景束状荆芥DC。是一种本地药用植物,属于Capparaceae科,发现于肯尼亚内罗毕的Nyandarua县和非洲的许多地方。它是一种灌木,其根传统上用于治疗感冒。的目标。本研究的目的是研究花楸不同部位溶剂提取物的抑菌活性,表征最有效提取物的植物化学成分,并鉴定最有效的化合物。研究的地点和时间。所有实验均在肯尼亚内罗毕肯雅塔大学化学系和微生物系进行。方法。采用碟式扩散法和管式稀释法对束束草叶、茎皮和根皮的石油醚、乙酸乙酯、甲醇和水提取物进行筛选,筛选出革兰氏阳性菌(金黄色葡萄球菌和枯草芽孢杆菌)和革兰氏阴性菌(鼠伤寒沙门菌和大肠杆菌)。采用柱层析法对活性最强的粗提物进行分离,并与活性最强的粗提物一起对所选菌株进行筛选。对活性最强的部分进行进一步的分馏,并对这些亚组分进行抗菌筛选,以测试亚组分与其成分之间可能的协同作用。然后用GC-MS和LC-ESI-MS方法对活性部位进行分析,确定主要成分。结果。藤皮乙酸乙酯提取物(CFR2)具有显著的体外抑菌活性。在获得的CFR2的7个分数中,分数2 (F2)的MIC值最低,因此最活跃。此外,F2被发现比从它得到的四个亚组分更有活性。这表明F2的成分协同作用。组分2含有酚类、萜烯和类黄酮。其中2个化合物经GC-MS鉴定为2,4-二叔丁基苯酚和(E,E)-2,4-十二烯醛;3个化合物经LC-ESI-MS鉴定为丹参酮II A、隐丹参酮和丹参素。结论。研究发现,CFR2是对细菌最具活性的提取物,表明大部分抗菌化合物集中在束草根中。后续的研究是针对色谱分离,以获得其他化学成分和筛选它们对各种菌株的细菌。
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引用次数: 0
Salting-Out Assisted Liquid-Liquid Extraction of Cr (VI) from Water Samples before Its Determination by UV-Vis Spectrophotometry 紫外-可见分光光度法测定水样中铬(VI)的盐析辅助液-液萃取
4区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-10-30 DOI: 10.1155/2023/8857010
Jote Dame, Feyisa Wedajo, Guyo Jilo Molole, Abera Gure
This paper proposes salting-out assisted liquid-liquid extraction for selective extraction of a Cr (VI)-1,5-diphenylcarbazide complex before its determination by UV-Vis spectrophotometry. Parameters affecting the complexation process and the extraction efficiency of the method were studied. The highest extraction efficiency was obtained when acetonitrile was used as an extraction solvent and (NH4)2SO4 was used as a salting-out agent. Under optimum conditions, the calibration curve constructed at seven concentration points exhibited good linearity from 0.015 to 2.00 mg/L with a 0.9973 coefficient of determination. The method’s detection and quantification limits were 0.004 and 0.015 mg/L, respectively. The method showed a 5.8 enrichment factor. The intra- and inter-day precisions studied at two concentration levels (0.75 and 1.25 mg/L) showed relative standard deviation values of <9.0. The recoveries of the spiked water samples at the two concentration levels ranged from 88.0 ± 2.5 to 97.3 ± 0.1%. The method demonstrated negligible interferences (<5%) for Fe, Cu, V, and Cd up to 500 mg/L. The findings showed that the method is simple, rapid, efficient, and selective to be used as an alternative procedure for analyzing Cr (VI) from water and other related matrices.
在紫外可见分光光度法测定Cr (VI)-1,5-二苯脲络合物前,采用盐析辅助液-液萃取法对络合物进行选择性萃取。研究了影响络合过程和萃取效率的参数。以乙腈为萃取溶剂,以(NH4)2SO4为盐析剂,萃取效率最高。在最佳条件下,7个浓度点的标定曲线在0.015 ~ 2.00 mg/L范围内线性良好,测定系数为0.9973。方法的检测限为0.004 mg/L,定量限为0.015 mg/L。该方法的富集系数为5.8。两种浓度水平(0.75和1.25 mg/L)下的日内和日间精密度的相对标准偏差值为<9.0。加样回收率在88.0±2.5 ~ 97.3±0.1%范围内。该方法对高达500mg /L的Fe, Cu, V和Cd的干扰可以忽略不计(<5%)。结果表明,该方法简便、快速、高效、选择性好,可作为分析水及其他相关基质中Cr (VI)的替代方法。
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引用次数: 0
Bioconvection Flow in the Presence of Casson Nanoparticles on a Stretching/Shrinking Vertical Sheet with Chemical Reaction 卡森纳米颗粒在拉伸/收缩垂直薄片上的生物对流流动与化学反应
4区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-10-26 DOI: 10.1155/2023/6199200
B. Arun, M. Deivanayaki, Selvakumar Kuppusamy Vaithilingam
A Casson nanoparticle is used in this study to investigate the effects of toxic reactions, temperatures, and concentrations on convective heat transfer flow across a stretching/shrinking vertical sheet. The goal is to convert the control linear partial differential equations (PDEs) into an ordinary differential equations (ODEs) set and analyses them statistically using the Bvp4c technique in MATLAB software. It is necessary to look how various variables, such as the Casson nanofluid measurement, the chemical change constants and Prandtl numbers, the concentration-thermal-buoyancy ratio, the microorganism-to-thermal-buoyancy rate of return, the Lewis number, and other bioconvection-related parameters (such as the variation in micro-organism concentration and the buoyancy parameter), affect each other. The numerical results of the velocity, temperature, concentration, and bioconvection flow profiles are displayed.
在这项研究中,卡森纳米颗粒被用于研究有毒反应、温度和浓度对拉伸/收缩垂直薄片上的对流换热流的影响。目标是将控制线性偏微分方程(PDEs)转化为常微分方程(ode)集,并在MATLAB软件中使用Bvp4c技术对其进行统计分析。有必要研究各种变量,如卡森纳米流体测量、化学变化常数和普朗特数、浓度-热-浮力比、微生物-热-浮力返回率、刘易斯数和其他与生物对流相关的参数(如微生物浓度和浮力参数的变化)如何相互影响。显示了速度、温度、浓度和生物对流流场的数值结果。
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引用次数: 0
Nanomaterials for Targeted Drug Delivery through Skin to Treat Various Diseases: Recent Trends and Future Perspective 用于皮肤靶向药物递送治疗各种疾病的纳米材料:最新趋势和未来展望
4区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-10-17 DOI: 10.1155/2023/3861758
Nazish Mumtaz, Muhammad Imran, Ayesha Javaid, Shoomaila Latif, Nazim Hussain, Liviu Mitu
There is an increased trend of drug delivery via skin due to its convenience and affordability. To accomplish this task in a better way and more successfully, nanotechnology has opened the door to transport drugs for the treatment of acute diseases in unique ways. For partially solvable drugs especially, designing new drug transportation systems is always challenging. However, it has been fixed by utilizing nanomaterials as effective carriers for drugs. These carriers allow the controlled and continuous drug release at the specific spotted site and have been successfully manipulated for the creation of innovative drug-delivery systems. These innovative systems are applied to overcome the challenge of reduced water solubility that may improve the drug accessibility, sustained release, and high metabolic stability. The prime emphasis of this review is particularly on the universal routes of drug administration through the skin, limitations of conventional drug delivery systems (DDS), and types and properties of nanomaterials (NMs) used. Recent advancements in NMs such as carbon-based NMs, inorganic-/metal-based NMs, polymeric NMs, and hybrid NMs for drug delivery and their mode of action have been summarized. This review further discusses existing constraints and difficulties that impede the integration of nanomaterials from research to practice, as well as recommendations for more efficient use of nanomaterials in a number of diseases.
由于皮肤给药的方便性和可负担性,有增加的趋势。为了更好、更成功地完成这项任务,纳米技术为以独特的方式运输治疗急性疾病的药物打开了大门。特别是对于部分可溶药物,设计新的药物输送系统一直是一个挑战。然而,利用纳米材料作为药物的有效载体已经解决了这个问题。这些载体允许药物在特定位点的受控和连续释放,并已成功地用于创新药物递送系统的创建。这些创新的系统被用于克服水溶性降低的挑战,从而改善药物的可及性、缓释和高代谢稳定性。这篇综述的主要重点是通过皮肤给药的通用途径,传统给药系统(DDS)的局限性,以及所使用的纳米材料(NMs)的类型和性质。综述了近年来碳基纳米材料、无机/金属基纳米材料、聚合物纳米材料和杂化纳米材料在药物传递和作用方式方面的研究进展。这篇综述进一步讨论了阻碍纳米材料从研究到实践整合的现有限制和困难,以及在一些疾病中更有效地使用纳米材料的建议。
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引用次数: 0
Extracellular Synthesis of Iron Oxide Nanoparticles Using an Extract of Bacillus circulans: Characterization and In Vitro Antioxidant Activity 利用环状芽孢杆菌提取物胞外合成氧化铁纳米颗粒:表征和体外抗氧化活性
4区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-10-16 DOI: 10.1155/2023/4659034
Ghulam Rabani, Muhammad Dilshad, Aamir Sohail, Aqsa Salman, Saba Ibrahim, Iqra Zafar, Hafiz Muhammad Arshad
This study explores the biosynthesis of iron oxide nanoparticles (IONPs) using Bacillus circulans bacterial supernatant as an inexpensive and sustainable alternative to traditional synthesis approaches. The resulting nanoparticles were found to have a uniform size distribution and a spherical shape and agglomerated to form clusters as observed through scanning electron microscopy (SEM). The average diameter of IONPs determined using SEM was 18.37 nm. Characterization using energy-dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD) confirmed the synthesis of maghemite (γ-Fe2O3) nanoparticles, with a crystallite size of 13.84 nm. Fourier-transform infrared spectroscopy (FT-IR) revealed the surface functional groups of IONPs. Additionally, the IONPs were evaluated for antioxidant activity using the DPPH and ABTS assays, displaying 39.44% inhibition of ABTS radical cations and 35.44% DPPH scavenging. Calcination of IONPs for two hours at 300°C resulted in the conversion to the hematite (α-Fe2O3) phase, with a crystallite size of 23.18 nm, and slightly lower antioxidant activity, 35.04% inhibition of ABTS radical cations, and 26.5% DPPH scavenging.
本研究探讨了利用环状芽孢杆菌细菌上清液作为传统合成方法的廉价和可持续的替代方法来生物合成氧化铁纳米颗粒(IONPs)。通过扫描电子显微镜(SEM)观察到,所得纳米颗粒具有均匀的尺寸分布和球形,并聚集形成团簇。扫描电镜测得离子束的平均直径为18.37 nm。利用能量色散x射线能谱(EDX)和x射线衍射(XRD)进行表征,证实合成了磁赤铁矿(γ-Fe2O3)纳米颗粒,晶粒尺寸为13.84 nm。傅里叶变换红外光谱(FT-IR)揭示了离子的表面官能团。此外,利用DPPH和ABTS实验评估了IONPs的抗氧化活性,显示出39.44%的ABTS自由基抑制和35.44%的DPPH清除。IONPs在300℃下煅烧2小时,转化为赤铁矿(α-Fe2O3)相,晶粒尺寸为23.18 nm,抗氧化活性略低,对ABTS自由基阳离子的抑制作用为35.04%,对DPPH的清除作用为26.5%。
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引用次数: 0
Retracted: Optimization of Flash Extraction of Akebia trifoliata Seed Oil by the Box-Behnken Response Surface Methodology and Comparison of Oil Yields from Different Origins Box-Behnken响应面法优化三叶草种子油闪提工艺及不同产地油收率比较
4区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2023-10-11 DOI: 10.1155/2023/9897156
Journal of Chemistry
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引用次数: 0
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