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A Novel Method Development and Validation by Ultra-Performance Liquid Chromatography for Assay of Asciminib in Dosage Form 超高效液相色谱法测定阿西米尼剂型的方法建立及验证
Q3 Chemistry Pub Date : 2023-05-31 DOI: 10.18596/jotcsa.1228364
Pridhvi Krishna GADDEY, Raja SUNDARARAJAN
The main objective of the present study was to develop and validate simple, precise, sensitive and accurate UPLC method for the estimation of asciminib in pure and dosage form. The UPLC method was developed by using Waters Acquity liquid chromatographic system and Zorbax Phenyl (100x1.0mm,1.7µm) column. The developed method was validated according to the international conference on harmonization (ICH) guidelines. The chromatographic separation of asciminib with good resolutions has been achieved by using the mobile phase acetonitrile: ammonium dihydrogen phosphate buffer (20:80 v/v) at a flow rate of 0.5 mL/min, injection volume of 5 µL, and at 242 nm wavelength. The validated method was found to be linear in the range of 4 - 60 µg/mL. The limit of detection (LOD) and limit of quantification (LOQ) for asciminib were found to be 0.4 and 0.12 µg/mL respectively. The % RSD was found to be less than 2 % revealing the precision of the developed method. Besides, the recovery rate was observed close to 100 % confirming the accuracy of the method. Minor alterations in the chromatographic conditions have revealed robustness and ruggedness of the developed method. The developed analytical method is simple, precise, sensitive, and reproducible which can be used for the estimation of asciminib.
本研究的主要目的是建立和验证一种简便、精确、灵敏、准确的超高效液相色谱(UPLC)方法,用于阿西米尼的纯度和剂型的测定。采用Waters Acquity液相色谱系统和Zorbax Phenyl (100 × 1.0mm,1.7µm)柱建立UPLC。根据国际协调会议(ICH)指南对所开发的方法进行了验证。采用流动相乙腈:磷酸二氢铵缓冲液(20:80 v/v),流速为0.5 mL/min,进样量为5µL,波长为242 nm,实现了阿西米尼的色谱分离,分离效果良好。该方法在4 ~ 60µg/mL范围内呈线性关系。阿西米尼的检出限和定量限分别为0.4和0.12µg/mL。RSD < 2%,表明该方法的精密度较高。回收率接近100%,证实了该方法的准确性。色谱条件的微小变化显示了所开发方法的稳健性和耐用性。该方法简便、准确、灵敏、重现性好,可用于阿西米尼的含量测定。
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引用次数: 0
Cytarabine determination from urine for Toxicokinetic and Excretion studies by High- Performance Liquid Chromatography-Tandem Mass Spectrometry 高效液相色谱-串联质谱法测定尿中阿糖胞苷的毒性动力学和排泄研究
Q3 Chemistry Pub Date : 2023-05-31 DOI: 10.18596/jotcsa.1190202
İbrahim DANİŞ, Ayşegül GÖLCÜ, Durişehvar ÜNAL
Cytarabine (Cyt) (also known as cytosine arabinoside (ara-C)) used in the treatment of acute myeloid leukemia (AML), acute lymphocytic leukemia (ALL). CYT applied in high doses for treatment can cause renal failure. Monitoring excreted urine drug levels can help kidney failure. For this reason, a method was developed and validated by HPLC-MSMS for urine CYT analysis, which is not included in the literature. In this study, a liquid chromatography (HPLC) with triple quadrupole Mass Spectrometric (MS/MS) method developed for the determination of Cyt from urine for toxicokinetic evaluation. Positive MRM mode selected for the quantification of Cyt. The product and major fragment ion for Cyt 244.0 &gt; 112.0 m/z, for IS 198.0 &gt; 152.0 m/z. The optimal MS parameters for Cyt and IS are as follows Fragmentor 80 V, 70 V, Collision energy, 6, 9 respectively. A novel simple, high-throughput and highly sensitive HPLC-MS/MS method was successfully developed and validated for the determination of Cyt from urine. The developed method has a simple one-step extraction method and a short run time (2.0 minutes) for analysis. The proposed method could be practical and reliable for excretion and toxicokinetic studies and as well as the Therapeutic Drug Monitoring study in humans without an invasive route for Cyt.
阿糖胞苷(Cyt)(又称阿糖胞苷(ara-C))用于治疗急性髓性白血病(AML)、急性淋巴细胞白血病(ALL)。高剂量CYT用于治疗可引起肾功能衰竭。监测排出尿液的药物水平可以帮助治疗肾衰竭。因此,我们开发了一种尿液CYT分析的方法,并通过HPLC-MSMS进行了验证,该方法未在文献中包含。本研究建立了一种液相色谱-三重四极杆质谱(MS/MS)法测定尿液中Cyt的毒性动力学评价方法。选择阳性MRM模式定量Cyt。Cyt 244.0的产物和主要片段离子;112.0 m/z,适用于IS 198.0 >152.0 m / z。Cyt和IS的最佳MS参数分别为Fragmentor 80 V, 70 V, Collision energy, 6, 9。建立了一种简便、高通量、高灵敏度的高效液相色谱-质谱联用(HPLC-MS/MS)测定尿液中Cyt的方法。该方法一步提取方法简单,分析运行时间短(2.0分钟)。该方法对于人体排泄和毒性动力学研究以及治疗性药物监测研究具有实用性和可靠性,无需侵入性Cyt途径。
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引用次数: 0
Physical and Spectroscopic Characterization of the Microcrystalline Cellulose Derivatives from Corn Cob and Daniella Oliveri Wastes 玉米芯和牛尾草废料微晶纤维素衍生物的物理和光谱表征
Q3 Chemistry Pub Date : 2023-02-28 DOI: 10.18596/jotcsa.1107627
Mariam Temitope BAKER, Olubunmi Stephen OGUNTOYE
Cellulose was extracted from wood dust waste samples of Daniella oliveri and corn cobs by acetic acid and alkaline pretreatment methods, while microcrystalline cellulose (MCC) derivative was produced by acid hydrolysis in 2 M HCl. The samples were tested for pH, moisture content, swelling capacities and ash contents. The data obtained were compared with those of commercial MCCs found in the literature. The functional groups in the microcrystalline cellulose derivatives was confirmed by the Fourier transform infrared (FTIR) spectroscopic method with characteristic absorption bands of;–OH stretching at 3416 cm-1; C-H stretching at 2918 cm-1; -OH bending at 1377 cm-1; 1159 cm-1; and C-O-C pyranose ring skeletal vibrations at 1026-1033 cm-1. The crystallinity absorption bands appeared at 1436 and 850 cm-1. The characteristic morphological features were established by scanning electron microscopy (SEM). Furthermore, the crystallinity of the microcrystalline cellulose was further confirmed using the X-ray powder diffraction (X-RD) technique, which showed three main reflections at 2θ=14.70°, 22.09°, and 34.24°.These results supported that microcrystalline cellulose derivative as cellulose I type and the acid pretreatment did not affect the structure of the MCC. The crystallinity indices were 69.3 and 73.2%, respectively. Daniella Oliveri and corn cob microcrystalline cellulose are, therefore, potential materials for further processing.
采用醋酸法和碱法分别从大牛和玉米芯木屑废样中提取纤维素,在2 M HCl中酸水解制备微晶纤维素衍生物。测试了样品的pH值、水分含量、膨胀能力和灰分含量。所得数据与文献中发现的商用mcc数据进行了比较。用傅里叶变换红外光谱法确定了微晶纤维素衍生物中的官能团,其特征吸收带为:-OH,在3416 cm-1处拉伸;C-H在2918 cm-1处的拉伸;- 1377 cm-1弯曲1159 cm - 1;C-O-C吡喃糖环骨架振动在1026-1033 cm-1。在1436和850 cm-1处出现结晶性吸收带。通过扫描电镜(SEM)确定了其特有的形态特征。此外,利用x射线粉末衍射(X-RD)技术进一步证实了微晶纤维素的结晶度,该微晶纤维素在2θ=14.70°、22.09°和34.24°处有三个主要反射。这些结果表明微晶纤维素衍生物为I型纤维素,酸处理对MCC的结构没有影响。结晶度指数分别为69.3和73.2%。因此,Daniella Oliveri和玉米芯微晶纤维素是进一步加工的潜在材料。
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引用次数: 0
Sorption of Cobalt and Nickel on Narcissus Tazetta L. Leaf Powder 水仙叶粉对钴和镍的吸附
Q3 Chemistry Pub Date : 2021-05-29 DOI: 10.18596/JOTCSA.881291
Süleyman İnan, Bekir Özkan
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引用次数: 2
Functionalized Sepiolitic Clay Nanofibers as a Natural Ingredient in Medical Cosmetics 功能化海泡石粘土纳米纤维作为医用化妆品的天然成分
Q3 Chemistry Pub Date : 2021-03-06 DOI: 10.18596/JOTCSA.847163
B. Benli, Ecehan Gönül
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引用次数: 0
Monoamine Oxidase Inhibitory Effects of Medicinal Plants in Management of Alzheimer's Disease 药用植物对阿尔茨海默病的抑制作用
Q3 Chemistry Pub Date : 2021-02-28 DOI: 10.18596/JOTCSA.823874
Tuba Ege, Hayriye Deniz Şelimen
Alzheimer's disease is the most common progressive neurodegenerative disorder that effects large population of society especially elderly people. Environmental and/or genetic factors contribute Alzheimer's disease to become a pivotal health problem but this relationship remains ambiguous. Globally growing prevalence of Alzheimer’s disease requires to understand cellular pathways that lead to Alzheimer’s disease and to develop new strategies for prevention and treatment. Elevated monoamine oxidase (MAO) enzymes activity with ages is associated with etiology of Alzheimer's disease. Inhibition of monoamine oxidase enzyme can protect from neuronal damage, thus it become one of the key pathway for management of Alzheimer’s disease. Using bioactive compounds from medicinal plants as potential monoamine oxidase inhibitors might be a better solution considering undesired side effects of synthetic drugs on human body. The purpose of this review is to implicate the importance of pharmacophore analysis which explains pharmacological properties of medicinal plants and interaction of bioactive compound from plants with MAO enzyme.
阿尔茨海默病是最常见的进行性神经退行性疾病,影响着大量社会人群,尤其是老年人。环境和/或遗传因素促使阿尔茨海默病成为一个关键的健康问题,但这种关系仍然模糊不清。阿尔茨海默病在全球范围内日益流行,需要了解导致阿尔茨海默病的细胞途径,并制定新的预防和治疗策略。随着年龄的增长,单胺氧化酶(MAO)活性的升高与阿尔茨海默病的病因有关。抑制单胺氧化酶可以保护神经元免受损伤,因此它成为治疗阿尔茨海默病的关键途径之一。考虑到合成药物对人体的不良副作用,使用药用植物中的生物活性化合物作为潜在的单胺氧化酶抑制剂可能是一个更好的解决方案。这篇综述的目的是暗示药效团分析的重要性,它解释了药用植物的药理学特性以及植物活性化合物与MAO酶的相互作用。
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引用次数: 4
Analysis of Trace Elements, Anticholinesterase Activity and ADME/Tox Profiling of some Achillea Species 部分Achillea属植物的微量元素、抗胆碱酯酶活性及ADME/Tox图谱分析
Q3 Chemistry Pub Date : 2021-02-28 DOI: 10.18596/JOTCSA.849654
D. Taşkın, T. Şahin, Mücahit Özdemir, B. Yalçın
In this study, the anti-cholinesterase activities of different extracts of Achillea lycaonica, A. vermicularis and A. nobilis L. subsp. neilreichii (Kerner) Formanek species were examined and then trace elements (Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Cd, and Pb) of the plants were analysed by ICP-MS. The pharmacokinetic properties of the phenolic compounds of these plants previously analyzed by us and the ADME-Tox (absorption, distribution, metabolism, excretion, and toxicity) profiles of the trace elements we identified in this study were estimated. According to the data obtained, it was determined that all three plants showed high acetyl-cholinesterase inhibition activity. The concentration of trace elements was lower than that declared by WHO, except for the A. lycaonica. It was determined that V, Cr, Fe, Co, and As metals in A. lycaonica exceeded the limit values determined by WHO. According to ADMET estimates, it is thought that the toxic values of all three plants are not high, and therefore the use of A. nobilis and A. vermicularis plants does not pose any health risk but A lycaonica should be used carefully due to the heavy metals.
本研究对水蛭、蛭毛草和野水蛭不同提取物的抗胆碱酯酶活性进行了研究。以neilreichii (Kerner) Formanek属植物为研究对象,采用电感耦合质谱法(ICP-MS)分析了植物的微量元素(Al、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Se、Cd和Pb)。我们分析了这些植物中酚类化合物的药代动力学特性,并对本研究中发现的微量元素的ADME-Tox(吸收、分布、代谢、排泄和毒性)谱进行了估计。根据所获得的数据,确定这三种植物都具有较高的乙酰胆碱酯酶抑制活性。各微量元素的浓度均低于WHO的标准,其余均低于WHO的标准。经测定,青花中V、Cr、Fe、Co、As等金属均超过WHO规定的限量值。根据ADMET的估计,人们认为这三种植物的毒性值都不高,因此使用牛蒡和蛭状牛蒡不会造成任何健康风险,但由于含有重金属,应谨慎使用牛蒡。
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引用次数: 0
Phytochemical Screening and Antibacterial Activity of Pistacia atlantica and Pinus canariensis Extracts 黄连木和金丝雀松提取物的植物化学筛选及其抗菌活性
Q3 Chemistry Pub Date : 2021-02-17 DOI: 10.18596/JOTCSA.836074
Obaida Alhajali, Adnan Ali-Nizam
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引用次数: 2
Corrosion Inhibitive Potentials Of (E)-5-((4-Benzoylphenyl)Diazenyl)-2-Hydroxybenzoic Acid On Mild Steel Surface In 0.5 M HCl- Experimental And DFT Calculations (E)-5-((4-苯甲酰基苯基)二氮基)-2-羟基苯甲酸在0.5M盐酸中对软钢表面的缓蚀电位-实验和DFT计算
Q3 Chemistry Pub Date : 2021-01-30 DOI: 10.18596/JOTCSA.821488
J. Amoko, O. Akinyele, O. Oyeneyin, Dare Olayanju
One of the ways of reducing metal corrosion and its devastating effects is by using organic corrosion inhibitors. This is because of the π-conjugation in their moieties, their ability to donate electrons to the metal’s vacant d-orbitals, and their low lying LUMO orbitals for accepting electrons as well from the metal, all these improve their adsorption on the metal surface. (E)-5-((4-benzoylphenyl)diazenyl)-2-hydroxybenzoic acid (AD4) was synthesized via the coupling reaction of p-aminobenzonephenone and Salicylic acid, characterized via FTIR, UV/Vis, 1H-NMR, and 13C-NMR spectroscopy. The melting point of AD4 is 103oC–106oC indicating that it is thermally stable and pure. Gravimetric and potentiodynamic polarization techniques were employed to obtain the corrosion rates (Cr) and percentage inhibition efficiency (%IE) at different concentrations of the inhibitor and at different temperatures. The thermodynamic parameters like Enthalpy, ∆Hoads, Entropy, ∆Soads and free energy of adsorption (∆Gads) of Adsorption were calculated. The Langmuir adsorption isotherm was used to describe the adsorption of AD4 molecules on mild steel. Quantum mechanical calculations were employed to calculate the electronic properties and global reactivity descriptors of AD4. The theoretical results are broadly consistent with experimental results. From the results obtained AD4 could be used as a corrosion inhibition agent in the oil and gas industries.
减少金属腐蚀及其破坏性影响的方法之一是使用有机缓蚀剂。这是因为它们部分的π-共轭,它们向金属的空位d轨道提供电子的能力,以及它们接受来自金属的电子的低位LUMO轨道,所有这些都改善了它们在金属表面的吸附。(E) 通过对氨基苯并霞石酮与水杨酸的偶联反应合成了-5-(4-苯甲酰基苯基)二氮烯基)-2-羟基苯甲酸(AD4),并用FTIR、UV/Vis、1H-NMR和13C-NMR对其进行了表征。AD4的熔点为103oC–106oC,表明其热稳定且纯净。采用重量法和动电位极化法测定了不同浓度缓蚀剂和不同温度下的腐蚀速率(Cr)和缓蚀率(%IE)。计算了吸附的焓、∆Hoads、熵、∆Soads和吸附自由能(∆Gads)等热力学参数。用Langmuir吸附等温线描述了AD4分子在软钢上的吸附。采用量子力学计算方法计算了AD4的电子性质和全局反应性描述符。理论结果与实验结果基本一致。从所获得的结果来看,AD4可以用作石油和天然气工业中的缓蚀剂。
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引用次数: 9
Calcined Eggshell for Removal of Victoria Blue R Dye from Wastewater Medium by Adsorption 煅烧蛋壳吸附法去除废水介质中维多利亚蓝R染料
Q3 Chemistry Pub Date : 2020-11-11 DOI: 10.18596/jotcsa.760083
İ̇lknur Tosun Satir, Kadir Erol
In this study, the use of calcined eggshell (CE) as an adsorbent in removing Victoria Blue R (VBR) dyestuff from the solution medium was investigated. For this purpose, pH, interaction time, adsorbate concentration, amount of adsorbent, and salt effect parameters were studied to determine the appropriate adsorption conditions. The highest adsorption yield was obtained at pH 2, 2.0 g/L adsorbent, and a stirring time of 5 minutes. 97% of the dye was removed under optimum adsorption conditions. The results obtained from the experimental studies showed that the adsorption mechanism is compatible with the pseudo-second-order kinetic model and the Langmuir isotherm model. SEM and IR analysis were performed for the characterization of CE.
本研究采用煅烧蛋壳(CE)作为吸附剂从溶液介质中去除维多利亚蓝R(VBR)染料。为此,研究了pH、相互作用时间、吸附质浓度、吸附剂用量和盐效应参数,以确定合适的吸附条件。在pH为2、吸附剂浓度为2.0g/L、搅拌时间为5分钟的条件下,吸附率最高。在最佳吸附条件下,染料去除率达97%。实验结果表明,该吸附机理符合拟二阶动力学模型和Langmuir等温线模型。用扫描电镜和红外光谱对CE进行了表征。
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引用次数: 8
期刊
Journal of the Turkish Chemical Society, Section A: Chemistry
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