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Determination of vitamins B1 and B6 in infant formula and food supplement samples using magnetic layered double hydroxide nanoadsorbent before liquid chromatography-tandem mass spectrometry 液相色谱-串联质谱法测定婴幼儿配方奶粉和食品补充剂样品中维生素B1和B6
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2022-12-14 DOI: 10.1080/10826076.2023.2192282
M. Zamani-Kalajahi, Ali Abolhassani, Samin Hamidi, M. Nemati
Abstract A magnetic Mg/Fe layered double hydroxide (magnetic LDH) nanocomposite was successfully prepared and used as a suitable adsorbent to simultaneously extract vitamins B1 and B6 from complex infant formula and food supplements. The important parameters affecting the extraction were optimized and the final parameters are as follows; the amount of adsorbent (20 mg), extraction time (6 min), elution time (8 min), and elution solvent ethanol in 750 µL. As-prepared nanoadsorbent was successfully in magnetic solid phase extraction set-up with no hazardous solvents and extraction performed in 6 min. The structure of nanoadsorbnet is lamellar, providing a wide surface to extract the analytes. The quantification of the analytes was accomplished using the liquid chromatography-tandem mass (LC/MS-MS) technique. Under optimum extraction conditions, the linearity ranged from 4 to 1000 ng/mL (vitamin B1) and 20 to 1000 ng/mL (vitamin B6), and the correlation of coefficients (R2) was obtained better than 0.99. The intra-day (n = 3) and inter-day precisions (n = 3 working days) calculated in the form of percent relative standard deviations (%RSDs) were obtained below 10.20%. The proposed method was successfully practiced for analyzing vitamins B1 and B6 in several brands of infant formulas and food supplements. Graphical Abstract
制备了磁性Mg/Fe层状双氢氧化物(磁性LDH)纳米复合材料,并将其作为吸附剂用于同时提取复合婴儿配方奶粉和食品补充剂中的维生素B1和B6。对影响提取的重要参数进行了优化,最终参数为:吸附剂用量(20 mg),萃取时间(6 min),洗脱时间(8 min),洗脱溶剂乙醇为750µL。制备的纳米吸附剂在无有害溶剂的磁固相萃取装置中成功提取,萃取时间为6分钟。纳米吸附网的结构是层状的,为提取分析物提供了广阔的表面。采用液相色谱-串联质谱(LC/MS-MS)技术进行定量分析。在最佳提取条件下,维生素B1含量在4 ~ 1000 ng/mL、维生素B6含量在20 ~ 1000 ng/mL范围内呈线性关系,相关系数(R2)大于0.99。日内(n = 3)和日间精度(n = 3个工作日)以百分比相对标准偏差(% rsd)计算,均在10.20%以下。所提出的方法已成功用于分析几个品牌的婴儿配方奶粉和食品补充剂中的维生素B1和B6。图形抽象
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引用次数: 0
Simultaneous quantification of multiple active components of the ginkgo ketoester tablet when combined with donepezil in four biological matrices from an Alzheimer’s animal model: Evaluation of drug distribution patterns in vivo 银杏酮酯片与多奈哌齐在四种阿尔茨海默病动物模型生物基质中联合使用时多种活性成分的同时定量分析:体内药物分布模式的评估
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2022-10-02 DOI: 10.1080/10826076.2023.2182318
Wen-Xia Pi, Xiao-Yu Huan, Yushun Zhuang, Jing Zhang, Xu-qin Shi, Gui-Sheng Zhou
Abstract Ginkgo ketoester tablets (GT) and donepezil are clinically used in combination to treat Alzheimer’s disease (AD). This study aimed to investigate the anti-dementia effects of two drugs alone and in combination by monitoring the distribution patterns of their active components in different biological matrices. A practical analytical method was developed for simultaneously quantifying 38 active compounds in different matrices at trace levels using ultra-performance liquid chromatography coupled with triple-quadrupole linear ion-trap tandem mass spectrometry (UHPLC-MS2). Under optimized conditions, good chromatographic separation of the 38 target compounds was achieved within 14 min, with acceptable linearity, limits of detections and quantifications, precision, stability, and extraction recovery and matrix effects. The developed analytical method quantified the 38 active components in the brain, plasma, intestine, and intestinal contents of AD mice treated with GT alone, donepezil alone, and a combination of the two drugs. The result showed that the combination group had enhanced anti-dementia active compounds and reduced levels of toxic compounds entering the targeted tissues. These findings support the combined use of GT and donepezil for increasing anti-dementia treatment efficiency and reducing toxicity. The proposed UHPLC-MS2 strategy could be used to monitor the levels of active compounds from different biological matrices in future studies. Graphical Abstract
摘要银杏酮酯片(GT)联合多奈哌齐治疗阿尔茨海默病(AD)。本研究旨在通过监测两种药物的活性成分在不同生物基质中的分布模式,探讨两种药物单独使用和联合使用的抗痴呆作用。建立了超高效液相色谱-三重四极杆线性离子阱串联质谱(UHPLC-MS2)同时定量测定不同基质中38种微量活性化合物的实用分析方法。在优化条件下,38个目标化合物在14 min内实现了良好的色谱分离,线性度、检测限、定量限、精密度、稳定性、提取回收率和基质效应均良好。所开发的分析方法量化了单独使用GT、单独使用多奈哌齐以及两种药物联合治疗的AD小鼠脑、血浆、肠道和肠道内容物中的38种活性成分。结果表明,联合组具有增强抗痴呆活性化合物和降低进入目标组织的有毒化合物水平。这些发现支持GT和多奈哌齐联合使用可提高抗痴呆治疗效率并降低毒性。在未来的研究中,UHPLC-MS2策略可用于监测不同生物基质中活性化合物的水平。图形抽象
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引用次数: 0
Bioactive mushroom polysaccharides: The structure, characterization and biological functions 生物活性蘑菇多糖的结构、特性及生物学功能
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2022-10-02 DOI: 10.1080/10826076.2023.2182317
Solehah Mohd Rosdan Bushra, A. Nurul
Abstract Medicinal mushrooms are conventionally used in the traditional medicine to treat or prevent illnesses. Polysaccharides are an important component in the mushrooms, a major contributor in their biological properties, and have been extensively studied since the past two decades. Medicinal mushrooms contain a class of polysaccharide known as β-glucan that possesses various biological activities. However, there are also other polysaccharides types that have been described to possess therapeutic potentials but they are less popular than the β-glucan. This review summarizes related information correlated to the mushroom polysaccharide structure, isolation and characterization methods, and their roles in biological activities including immunomodulatory, anticancer, anti-inflammatory, antioxidant and anti-microbial properties. Graphical Abstract
药用蘑菇在传统医学中通常用于治疗或预防疾病。多糖是蘑菇的重要成分,是蘑菇生物学特性的主要贡献者,近二十年来被广泛研究。药用蘑菇含有一类被称为β-葡聚糖的多糖,具有多种生物活性。然而,也有其他类型的多糖被描述为具有治疗潜力,但它们不如β-葡聚糖受欢迎。本文综述了香菇多糖的结构、分离、表征方法及其在免疫调节、抗癌、抗炎、抗氧化、抗微生物等生物活性方面的研究进展。图形抽象
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引用次数: 1
An HP-TLC densitometric method and fingerprinting for estimating capecitabine and thymoquinone simultaneously and its application in nanoscience using Box–Behnken design 同时估算卡培他滨和胸腺嘧啶醌的HP-TLC密度法和指纹图谱及其在纳米科学中的应用
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2022-10-02 DOI: 10.1080/10826076.2023.2183867
Prasiddhi Raikar, P. Dandagi, Amruta Balekundri
Abstract World Health Organization estimates that 10% of medications are of inferior quality, thus dangerous to human health. One way to avoid such a problem is to create an adequate, economical, and competitive analytical system. As a result, the study’s goal is to create a High-Performance Thin Layer Chromatography (HP-TLC) method for determining capecitabine (CAP) and thymoquinone (TQ) simultaneously. To the best of our knowledge, no such method for determining CAP and TQ simultaneously exists today. The method was created by implementing an analytical quality-by-design approach based on the Box–Behnken design (BBD) to optimize the chromatographic conditions and a combination of factors such as toluene volume (A), solvent front (B), and chamber saturation time (C), all of which were likely to affect the R f of CAP and TQ, respectively, later validated using TLC-silica coated plate 60 F254. The validated parameters were within an acceptable range, according to ICH guidelines. BBD design revealed that the volume of toluene and solvent front had a greater effect on all of the responses studied and thus needs to be controlled. The developed method of the analysis was found to be facile, dependable, expeditious, cost-effective, and could be used to quantify CAP and TQ in Nanoformulation. Graphical Abstract RESEARCH HIGHLIGHTS To determine both the drugs in nanoformulation, an accelerated and expeditious densiometric HP-TLC method was developed and validated. Particle size, zeta potential, entrapment efficiency (EE), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM) analysis were all performed on the prepared nanoformulation. According to ICH guidelines, the developed method has been tested for linearity, range, detection limit, quantification limit, precision, and robustness. A review of the literature reveals that there are several methods for determining CAP and TQ individually but no HP-TLC method has been reported for simultaneous estimation of CAP and TQ in the combined dosage form. Changes in mobile phase volume and changes in chamber saturation duration showed percent RSD-within the 2% criterion, confirming the robustness of the developed method.
世界卫生组织估计,有10%的药品质量低劣,对人体健康造成危害。避免这种问题的一种方法是创建一个适当的、经济的、有竞争力的分析系统。因此,本研究的目的是建立同时测定卡培他滨(CAP)和百里醌(TQ)的高效薄层色谱(HP-TLC)方法。据我们所知,目前还没有这样的方法可以同时确定CAP和TQ。采用基于Box-Behnken设计(BBD)的分析质量设计方法,优化色谱条件和甲苯体积(a)、溶剂前沿(B)和腔室饱和时间(C)等因素的组合,分别影响CAP和TQ的R f,随后使用tlc -二氧化硅包覆板60 F254进行验证。根据ICH指南,验证参数在可接受范围内。BBD设计表明,甲苯和溶剂前沿的体积对所研究的所有反应都有较大的影响,因此需要控制。结果表明,该方法简便、可靠、快速、经济,可用于纳米制剂中CAP和TQ的定量分析。为了对两种药物的纳米制剂进行快速、快速的密度测定,建立了一种快速、快速的HP-TLC方法。对制备的纳米制剂进行了粒径、zeta电位、包封效率(EE)、扫描电镜(SEM)和透射电镜(TEM)分析。根据ICH指南,开发的方法已进行了线性,范围,检测限,定量限,精密度和鲁棒性测试。回顾文献发现,有几种方法可以单独测定CAP和TQ,但尚未有HP-TLC方法同时测定联合剂型中CAP和TQ的报道。流动相体积和腔室饱和时间变化的rsd均在2%的标准范围内,证实了该方法的鲁棒性。
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引用次数: 1
Development of a multivariate model with desirability-based optimization for simultaneous determination of five co-administrated drugs for the management of COVID-19 infection in their dosage forms via validated RP-HPLC method 通过经验证的反相高效液相色谱法同时测定五种用于治疗新冠肺炎感染的联合用药的多变量模型的开发
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2022-10-02 DOI: 10.1080/10826076.2023.2168691
S. T. Hassib, Marwa A. Moffid, N. A. Aly, E. Mostafa
Abstract More than 2.9 million people have died as a result of the global demographic impact of the coronavirus illness of 2019 (COVID-19). Numerous antiviral and anti-inflammatory medications have FDA approval to treat COVID-19 patients. For the simultaneous determination of COVID-19 utilized medications (Remdesivir, Moxifloxacin, Dexamethasone, Apixaban, and paracetamol) in their dosage forms, a sensitive technique has been developed and validated. The aforementioned medications were separated and quantified with the help of experimental design. The Box-Behnken design was used in the experiment to optimize the chromatographic method’s analytical parameters. It employed RP-HPLC with a UV detector. An INERTSIL ODS-3 C18 column (5 µm, 250 × 4.6 mm) with mobile phase composed of acetonitrile: 30 mmoL potassium dihydrogen phosphate buffer (pH = 7.5) (50:50, v/v), at room temperature was employed to separate the aforementioned drugs. Paracetamol was linear over the concentration range (1–50 µg/mL), Moxifloxacin (5–70 µg/mL), Apixaban (5–70 µg/mL), Dexamethasone (1–100 µg/mL), and Remdesivir (5–100 µg/mL). According to ICH guidelines, the new approach underwent thorough validation. Between the proposed method’s results and those from the reference or reported methods, there was no significant difference. The technique is simple to use in research of the cited medications in their dosage forms for quality control aspects. Graphical Abstract
2019年冠状病毒病(COVID-19)对全球人口造成的影响已导致290多万人死亡。许多抗病毒和抗炎药物已获得FDA批准用于治疗COVID-19患者。为了同时检测COVID-19所用药物(瑞德西韦、莫西沙星、地塞米松、阿哌沙班和扑热息痛)的剂型,开发并验证了一种敏感技术。通过实验设计对上述药物进行分离和定量。实验采用Box-Behnken设计优化色谱法的分析参数。采用反相高效液相色谱法,紫外检测器。采用INERTSIL ODS-3 C18色谱柱(5µm, 250 × 4.6 mm),流动相为乙腈:30 mmoL磷酸二氢钾缓冲液(pH = 7.5) (50:50, v/v),室温下分离上述药物。对乙酰氨基酚(1 ~ 50µg/mL)、莫西沙星(5 ~ 70µg/mL)、阿哌沙班(5 ~ 70µg/mL)、地塞米松(1 ~ 100µg/mL)、瑞德西韦(5 ~ 100µg/mL)在浓度范围内呈线性关系。根据ICH指南,新方法经过了彻底的验证。本文方法的结果与文献或报道方法的结果无显著差异。该方法简便,可用于对所引药物的剂型进行质量控制研究。图形抽象
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引用次数: 1
Glycolipids isolation and characterization from natural source: A review 天然来源糖脂的分离与表征综述
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2022-10-02 DOI: 10.1080/10826076.2023.2165097
A. Daku, S. B. Al-Mhanna, Ruzilawati Abu Bakar, A. Nurul
Abstract For centuries, many natural products are known to contain a wide range of glycolipid compounds; some are chemical substances that produce a definite biological/physiological effect. Isolation and characterization of glycolipids are evolving with new techniques being or under development. This review gives a brief description of different methods of natural glycolipids extraction, isolation, and characterization. Modern extraction instruments and techniques accelerate glycolipids’ extraction processes. Chromatographic methods, such as column chromatography and TLC are the most commonly used techniques for glycolipid isolation and purification, different characterization techniques ranging from chemical methods, reagents spray UV-detection, MS, FTIR, and NMR with later tandem-MS, TOF, FID, ESI, and ELSD modifications of the existing techniques allowing faster, more sensitive and direct analysis. Graphical Abstract
几个世纪以来,许多天然产物被认为含有广泛的糖脂化合物;有些是产生一定生物/生理效应的化学物质。随着新技术的出现和发展,糖脂的分离和表征也在不断发展。本文综述了天然糖脂提取、分离和表征的不同方法。现代提取仪器和技术加速了糖脂的提取过程。色谱方法,如柱层析和薄层色谱是糖脂分离和纯化最常用的技术,不同的表征技术包括化学方法,试剂喷雾紫外检测,质谱,FTIR和NMR,以及后来的串联质谱,TOF, FID, ESI和ELSD对现有技术的修改,使分析更快,更敏感和更直接。图形抽象
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引用次数: 0
Mechanism of the effect of Xiaoyao powder treatment on exercise capacity of depressed rats—A stable isotope tracer metabolomic study 逍遥散对抑郁大鼠运动能力影响的机制——稳定同位素示踪代谢组学研究
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2022-07-21 DOI: 10.1080/10826076.2022.2163499
Cui Ji, Weidi Zhao, Jie Zheng, Shi Zhou, Jun-sheng Tian, Yumei Han, Xuemei Qin
Abstract Depression accounts for 10% of the total global burden of nonfatal disease. Xiaoyao Powder, a well-known traditional Chinese medicine is commonly used to treat depression. However, its therapeutic mechanisms have not yet been fully elucidated. In this study, a rat depression model was established by the application of chronic unpredictable mild stress (CUMS). The depressed rats were randomly distributed to four groups: Blank Control, CUMS control, CUMS with Venlafaxine (a positive control) treatment, and CUMS with Xiaoyao Powder treatment, with 12 rats in each group. Depression behavioral and exercise tests were performed weekly during the four-week intervention. Stable isotope tracer metabolomics and molecular biology techniques were utilized to determine the changes in serum metabolites pre and post the intervention period, aiming to elucidate the mechanism of Xiaoyao Powder in improving the depression symptoms and exercise capacity of the depressed rats. The results found that the Xiaoyao Powder treatment significantly improved the performance in the behavioral and exercise tests, as well as affected the levels of metabolites, such as pyruvic acid, lactic acid, and citric acid in serum. It was concluded that Xiaoyao Powder intervention had a significant effect on the pyruvic acid metabolism, glycolysis/gluconeogenesis, and tricarboxylic acid cycle in the serum of the depressed rats, which could contribute to the understanding of the mechanism of the intervention. GRAPHICAL ABSTRACT
摘要抑郁症占全球非致命疾病总负担的10%。逍遥散是一种著名的中药,常用于治疗抑郁症。然而,其治疗机制尚未完全阐明。本研究采用慢性不可预测轻度应激(CUMS)建立大鼠抑郁模型。将抑郁大鼠随机分为空白对照组、CUMS对照组、文拉法辛治疗组和逍遥散治疗组,每组12只。在为期四周的干预期间,每周进行抑郁行为和运动测试。采用稳定同位素示踪代谢组学和分子生物学技术,测定干预前后血清代谢产物的变化,旨在阐明逍遥散改善抑郁大鼠抑郁症状和运动能力的机制。结果发现,逍遥散治疗显著改善了行为和运动测试的表现,并影响了血清中丙酮酸、乳酸和柠檬酸等代谢产物的水平。结论逍遥散干预对抑郁大鼠血清丙酮酸代谢、糖酵解/糖异生和三羧酸循环有显著影响,有助于了解干预机制。图形摘要
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引用次数: 2
Characterization of quality differences of Ophiopogonis Radix from different origins by TLC, HPLC, UHPLC-MS and multivariate statistical analyses 不同产地麦冬药材质量差异的TLC、HPLC、UHPLC-MS及多元统计分析
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2022-07-21 DOI: 10.1080/10826076.2022.2159977
Ling Jiang, Y. Qiu, Zhuliang Chen, Lunbo Luo, Hongxia Tang, Xudong Zhou, Hanwen Yuan, Wen Wang, Ping Liu
Abstract Ophiopogonis Radix is normally used as a traditional medicine and healthy food in China. Thin-layer chromatography (TLC), total saponin content analysis, high-performance liquid chromatographic (HPLC) fingerprinting, ultra-high-performance liquid chromatographic (UHPLC) tandem mass (MS) spectra and multivariate statistical analyses were used to analyze differences in quality of Ophiopogonis Radix from three main producing areas in China. The TLC spots of samples obtained from Zhejiang were clearer and darker than samples from Sichuan and Shandong. Additionally, HPLC fingerprinting analysis of 14 common peaks of the Ophiopogonis Radix samples indicated that the similarities of the 15 batches of samples were between 0.94 and 0.99. Finally, UPLC-Orbitrap MS analysis was used to identify the 13 common peaks of Ophiopogonis Radix. These results showed that Ophiopogonis Radix obtained from different regions can be distinguished well using a combination of analytical techniques, based on differences in their chemical components. The combination of these techniques allows comprehensive and reliable quality evaluation of Ophiopogonis Radix. This study provides references for determining the quality of Ophiopogonis Radix obtained from different regions, which will guide its use as medicine or food. GRAPHICAL ABSTRACT
摘要麦冬在中国是一种常用的中药和保健食品。采用薄层色谱(TLC)、总皂苷含量分析、高效液相色谱(HPLC)指纹图谱、超高效液相色谱(UHPLC)串联质谱(MS)和多元统计分析等方法,对中国3个主要产区麦冬药材的质量差异进行了分析。浙江产样品的TLC斑点比四川和山东产样品更清晰、颜色更深。另外,对15批麦冬样品的14个共有峰进行HPLC指纹图谱分析,相似度在0.94 ~ 0.99之间。最后,采用UPLC-Orbitrap质谱法对麦冬药材中的13个共有峰进行了鉴定。结果表明,不同产地麦冬药材的化学成分不同,综合分析方法可以很好地区分不同产地麦冬药材。综合这些技术,可以对麦冬进行全面、可靠的质量评价。本研究为不同产地麦冬药材质量的确定提供参考,指导麦冬药材和食品的使用。图形抽象
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引用次数: 1
Emerging trends in extraction and analytical techniques for bromelain 菠萝蛋白酶提取和分析技术的新趋势
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2022-07-21 DOI: 10.1080/10826076.2022.2161573
D. Maheshwari, J. Shah, Darshil Shah, Paresh K. Patel, Yash Raj Singh
Abstract Bromelain, a proteolytic enzyme isolated from the stem and fruit of Ananas comosus has gained tremendous importance as anti-inflammatory, anticancer, and fibrinolytic agent in the clinical field. Recent anti-cancer and anti-thrombolytic activity of Bromelain has opened new areas of research in the field of safety and efficacy. Bromelain is widely used since time immemorial alone and in combination with other drugs in the treatment of Rheumatoid Arthritis. The review aims to evaluate various extraction and analytical techniques employed for the assay of Bromelain in complex enzymatic mixtures which involves the use of diverse derivatizing agents with variable sensitivity and accuracy. The review focuses on homogenous and heterogenous techniques used for the estimation of Bromelain in the crude extract. This review also emphasizes on separation novel techniques, such as ion-exchange chromatography for isolation and purification of Bromelain supported by Gel Chromatography. This review also aims to provide deep insight into recent reverse micellar techniques employed as an effective tool for the purification of Bromelain. An overview of hyphenated bioanalytical techniques, such as LC-MS/MS for analysis of Bromelain in Plasma is also inculcated in the study. The techniques presented in the study provide diversified tools employed for the analysis of Bromelain in crude mixtures of complex enzymes of clinical significance. GRAPHICAL ABSTRACT
摘要菠萝蛋白酶是从Ananas comosus茎和果实中分离得到的一种蛋白水解酶,在临床上作为抗炎、抗癌和纤溶剂具有重要意义。近年来,菠萝蛋白酶的抗癌和抗血栓溶解活性在安全性和有效性领域开辟了新的研究领域。自古以来,菠萝蛋白酶就被广泛用于单独治疗类风湿性关节炎,并与其他药物联合治疗。本综述旨在评估用于测定复杂酶混合物中菠萝蛋白酶的各种提取和分析技术,其中包括使用不同灵敏度和准确性的衍生剂。综述了用于估算粗提取物中菠萝蛋白酶的同质和异质技术。本文还着重介绍了近年来分离菠萝蛋白酶的新技术,如离子交换色谱法和凝胶色谱法。这篇综述还旨在深入了解近年来反胶束技术作为纯化菠萝蛋白酶的有效工具。本研究还概述了联用生物分析技术,如LC-MS/MS分析血浆中菠萝蛋白酶。该研究中提出的技术为分析具有临床意义的复杂酶粗混合物中的菠萝蛋白酶提供了多种工具。图形摘要
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引用次数: 1
Characterization of the major degradation products of the praziquantel API by mass spectrometry: Development and validation of a stability-indicating reversed phase UPLC method API吡喹酮主要降解产物的质谱表征:稳定性指示反相UPLC方法的开发和验证
IF 1.3 4区 化学 Q3 Pharmacology, Toxicology and Pharmaceutics Pub Date : 2022-07-21 DOI: 10.1080/10826076.2022.2163253
Ajay Kumar, R. Chalannavar
Abstract Praziquantel was subjected to forced degradation studies under various conditions of hydrolysis (acidic, alkaline, and neutral/water), oxidation, photolysis, and thermal as prescribed by International Conference on Harmonization guideline Q1A (R2). A short and simple reversed phase UHPLC method was developed for the Praziquantel API. The method was developed on a Shimadzu, Shimpack Velox, SP-C18, 100 × 2.1 mm, 1.8 µm column. The isocratic mobile phase was a blend of water and acetonitrile in the ratio of 70:30 (v/v), respectively. The flow rate of the mobile phase was 0.5 mL/min. The developed method was validated using ICH guidelines. The parameters considered for method validation were solution stability, specificity, DL/QL, linearity, accuracy, precision, and robustness. The drug showed significant degradation in acidic and alkaline conditions while slight degradation was observed in water and oxidative conditions. The drug was found to be stable in photolytic and thermal conditions. The characterization of four major degradation products (DP1, DP2, DP3, and DP4) was done with LC–Q-TOF-MS/MS in combination with accurate mass measurements. The most probable mechanisms for the formation of DPs have been proposed on the basis fragmentation pattern. Graphical Abstract
摘要根据国际协调会议指南Q1A(R2)的规定,在水解(酸性、碱性和中性/水)、氧化、光解和热的各种条件下对吡喹酮进行了强制降解研究。针对API,开发了一种简单快捷的反相超高压可编程控制器方法。该方法是在Shimadzu,Shimpack Velox,SP-C18100上开发的 × 2.1 毫米,1.8 µm柱。等度流动相是水和乙腈的混合物,其比例分别为70:30(v/v)。流动相的流速为0.5 毫升/分钟。使用ICH指南对所开发的方法进行了验证。方法验证所考虑的参数包括溶液稳定性、特异性、DL/QL、线性、准确度、精密度和稳健性。该药物在酸性和碱性条件下表现出显著降解,而在水和氧化条件下观察到轻微降解。该药物被发现在光解和热条件下是稳定的。四种主要降解产物(DP1、DP2、DP3和DP4)的表征采用LC–Q-TOF-MS/MS结合准确的质量测量进行。根据碎片模式提出了最可能的DP形成机制。图形摘要
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引用次数: 1
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