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Isolation of highly polar galloyl glucoside tautomers from Saxifraga tangutica through preparative chromatography and assessment of their in vitro antioxidant activity 通过制备色谱法从虎杖中分离出高极性五倍子酰葡萄糖苷同系物并评估其体外抗氧化活性
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-08 DOI: 10.1186/s13065-024-01330-z
Yingying Tong, Ming Chu, Jia Zhou, Qilan Wang, Gang Li, A. M. Abd El-Aty, Jun Dang

In this work, the rapid and efficient preparation of isolated galloyl glucoside tautomer free radical inhibitors was investigated using Saxifraga tangutica as a raw material. Four highly polar galloyl glucoside tautomers, 3-O-galloyl-α-d-glucose ⇌ 3-O-galloyl-β-d-glucose (Fr2-1-1), 2-O-galloyl-α-d-glucose ⇌ 2-O-galloyl-β-d-glucose (Fr2-1-2/2-1-3), 1-O-galloyl-β-d-glucose (Fr2-2-1), and 6-O-galloyl-α-d-glucose ⇌ 6-O-galloyl-β-d-glucose (Fr2-3-1/Fr2-3-2), were obtained via two-step medium-pressure liquid chromatography (with solid loading instead of conventional liquid injection) and one-step high-performance chromatography coupled with on-line RPLC-DPPH techniques for targeted isolation. This separation integration technique not only increases sample intake and reduces time cost but also visualizes each step of targeted separation. All four compounds were isolated from the plant for the first time. In vitro antioxidant activity assays by DPPH (1,1‑diphenyl-2-picrylhydrazyl) revealed that Fr2-1-2/Fr2-1-3 (IC50: 5.52 ± 0.32 μM), Fr2-2-1 (IC50: 7.22 ± 0.57 μM), and Fr2-3–1/Fr2-3-2 (IC50: 7.36 ± 0.25 μM) had superior free radical scavenging abilities and that both were superior to that of quercetin (IC50: 18.61 ± 3.55 μM). Oxidative stress assays revealed that Fr2-1-2/Fr2-1-3 significantly inhibited oxidative stress damage in H2O2-induced HepG2 cells, decreased the level of ROS (P < 0.01) and protected hepatocytes. Combined with the current results, gallic acid showed greater antioxidant activity when H atoms were replaced at d-glucose –OH (C-2) than at the other three sites [–OH (C-1), –OH (C-6) and –OH (C-3)].

本研究以西洋参为原料,研究了如何快速高效地制备分离的五倍子酰葡萄糖苷同系物自由基抑制剂。四种高极性的五倍子酰葡萄糖苷同系物:3-O-galloyl-α-d-glucose ⇌ 3-O-galloyl-β-d-glucose(Fr2-1-1),2-O-galloyl-α-d-glucose ⇌ 2-O-galloyl-β-d-glucose(Fr2-1-2/2-1-3)、1-O-Galloyl-β-d-glucose (Fr2-2-1) 和 6-O-Galloyl-α-d-glucose ⇌ 6-O-Galloyl-β-d-glucose (Fr2-3-1/Fr2-3-2)、通过两步中压液相色谱法(用固体负载代替传统的液体进样)和一步高效色谱法结合在线 RPLC-DPPH 技术进行定向分离。这种分离集成技术不仅增加了样品量,降低了时间成本,而且还能直观地看到定向分离的每个步骤。所有四种化合物都是首次从该植物中分离出来。通过 DPPH(1,1-二苯基-2-苦基肼)体外抗氧化活性检测发现,Fr2-1-2/Fr2-1-3(IC50:5.52 ± 0.32 μM)、Fr2-2-1(IC50:7.22 ± 0.57 μM)、Fr2-3-1/Fr2-3-2(IC50:7.36 ± 0.25 μM)具有更强的自由基清除能力,均优于槲皮素(IC50:18.61 ± 3.55 μM)。氧化应激实验表明,Fr2-1-2/Fr2-1-3 能显著抑制 H2O2 诱导的 HepG2 细胞的氧化应激损伤,降低 ROS 水平(P < 0.01),保护肝细胞。结合目前的研究结果,与其他三个位点[-OH (C-1)、-OH (C-6)和-OH (C-3)]相比,没食子酸在二葡萄糖-OH (C-2)位点取代 H 原子时显示出更强的抗氧化活性。
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引用次数: 0
Application of nucleophilic substitution reaction for sensitive determination of heptaminol hydrochloride in pharmaceuticals 应用亲核取代反应灵敏测定药物中的盐酸庚胺醇
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-07 DOI: 10.1186/s13065-024-01327-8
Mahmoud Abdelgaleel, Dalia M. Nagi, Mohamed Oraby, Sayed M. Derayea, Pakinaz Y. Khashaba

A straightforward and sensitive spectrofluorimetric approach was established for the determination of heptaminol hydrochloride (HTM-HCl) based on the derivatization of the drug through its reaction with 5-dimethylaminonaphthalene-1-sulfonyl chloride (Dansyl chloride). The reagent underwent a nucleophilic substitution of its chlorine atom with HTM to give N-(5-dimethylaminonaphthalene-1-sulfonyl)-6-amino-2-methylheptan-2-ol. The highly luminescent derivative was extracted using methylene chloride and subjected to analysis at an excitation wavelength of 345 nm and an emission wavelength of 490 nm. The chemical reaction occurred within an aqueous environment buffered with a 0.1 M borate buffer solution adjusted to pH 10.5. Experimental findings indicate that the proposed method displays sensitivity and linearity across a concentration range from 0.03 to 2 µg mL− 1. The method achieves lower detection and quantification limits of 0.016 and 0.048 µg mL− 1, respectively. The analytical validation of this method followed the guidelines outlined by the International Council of Harmonization (ICH). This approach was applied effectively for quantifying the medication in both tablet and oral drops formulations available on the market, demonstrating excellent recovery of 98.95 ± 0.45 for tablets and 99.37 ± 0.24 for oral drops with no interference from excipients.

通过药物与 5-二甲基氨基萘-1-磺酰氯(丹酰氯)的衍生化反应,建立了一种测定盐酸庚胺醇(HTM-HCl)的简单灵敏的光谱荧光测定法。试剂的氯原子与 HTM 发生亲核取代反应,生成 N-(5-二甲基氨基萘-1-磺酰基)-6-氨基-2-甲基庚-2-醇。用二氯甲烷萃取这种高发光衍生物,并在 345 nm 的激发波长和 490 nm 的发射波长下进行分析。化学反应发生在 pH 值为 10.5 的 0.1 M 硼酸盐缓冲溶液缓冲的水环境中。实验结果表明,该方法在 0.03 至 2 µg mL- 1 的浓度范围内具有灵敏度和线性关系。该方法的检出限和定量限分别为 0.016 和 0.048 µg mL- 1。该方法的分析验证遵循了国际协调理事会(ICH)的指导方针。该方法可有效地定量检测市售片剂和口服滴剂中的药物含量,片剂的回收率为 98.95 ± 0.45,口服滴剂的回收率为 99.37 ± 0.24,且无辅料干扰。
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引用次数: 0
Development and validation of HPLC-UV and LC-MS/MS methods for the quantitative determination of a novel aminothiazole in preclinical samples 开发并验证用于定量测定临床前样品中一种新型氨基噻唑的 HPLC-UV 和 LC-MS/MS 方法
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-07 DOI: 10.1186/s13065-024-01321-0
Vinay N. Basavanakatti, Mohammad Ali, D.R. Bharathi, Sheikh Murtuja, Barij Nayan Sinha, Venkatesan Jayaprakash, Faiyaz Shakeel

Aminothiazoles are the important class of chemical groups which have proven their broad range of biological activities. A novel aminothiazole (21MAT) was quantified in analytical solutions using a high-performance liquid chromatography (HPLC) approach that was developed and partially validated for the analysis of in vitro experimental samples. An isocratic elution on reverse phase Phenomenex® Luna C18 (50 mm × 4.6 mm, 5 μm) column with 55% 0.1% v/v orthophosphoric acid in water and 45% of orthophosphoric acid in acetonitrile at a flow rate of 1 mL/min was used. The analyte was detected at 272 nm. Similar to this, a robust bioanalytical technique, LC-mass spectrometry (LC-MS/MS) was created and verified to measure 21MAT in rat plasma for use in in vitro screening study samples and early-stage pharmacokinetic research. The protein precipitation method was used to extract 21MAT from plasma. The mixture of 95: 5% v/v methanol: acetonitrile and 0.1% v/v formic acid, along with 15% of 5 mM ammonium formate solution, was used to separate the mixture on a reverse phase Waters Xterra RP® C18 (150 mm × 4.6 mm, 5 μm) column at a flow rate of 1 mL/min. Using electro spray ionisation mode in multiple reaction monitoring mode, the analyte and internal standard (a structural analogue) were both identified. According to current criteria, all validation parameters (specificity, selectivity, accuracy, precision, recovery, matrix factor, hemolysis effect, and stability) were evaluated in rat plasma. The area response of 21MAT was found to be linear over the concentration range of 1.25–1250 ng/mL in rat plasma. Both techniques are suitable for use in any format of preclinical research and were sufficiently reliable to measure 21MAT precisely in various matrices. In silico prediction helped in understanding absorption, distribution, metabolism, excretion, and toxicity (ADMET) behaviour of the molecule. Both developed LC-MS/MS and HPLC-UV methods were successfully used to quantify the analyte in in vitro screening study samples.

氨基噻唑是一类重要的化学物质,已被证明具有广泛的生物活性。本研究采用高效液相色谱法(HPLC)对分析溶液中的一种新型氨基噻唑(21MAT)进行了定量分析。采用反相 Phenomenex® Luna C18(50 mm × 4.6 mm,5 μm)色谱柱,以 55% 0.1% v/v 原磷酸水溶液和 45% 原磷酸乙腈水溶液进行等度洗脱,流速为 1 mL/min。在 272 纳米波长处检测分析物。与此类似,我们还创建并验证了一种稳健的生物分析技术--液相色谱-质谱法(LC-MS/MS),用于测量大鼠血浆中的 21MAT 含量,以用于体外筛选研究样本和早期药代动力学研究。采用蛋白质沉淀法从血浆中提取 21MAT。使用 95% v/v 甲醇:5% v/v 乙腈和 0.1% v/v 甲酸的混合溶液以及 15% 5 mM 甲酸铵溶液,在反相 Waters Xterra RP® C18(150 mm × 4.6 mm,5 μm)色谱柱上分离混合物,流速为 1 mL/min。在多反应监测模式下使用电喷雾离子化模式,对分析物和内标物(一种结构类似物)进行了鉴定。根据现行标准,在大鼠血浆中对所有验证参数(特异性、选择性、准确性、精密度、回收率、基质因子、溶血效应和稳定性)进行了评估。在大鼠血浆中 1.25-1250 纳克/毫升的浓度范围内,21MAT 的面积响应呈线性关系。这两种技术都适用于任何形式的临床前研究,而且在各种基质中精确测量 21MAT 都足够可靠。硅学预测有助于了解该分子的吸收、分布、代谢、排泄和毒性(ADMET)行为。所开发的 LC-MS/MS 和 HPLC-UV 方法均成功用于体外筛选研究样品中分析物的定量。
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引用次数: 0
Influence of physico-chemical properties of hydroxypropyl methylcellulose on quetiapine fumarate release from sustained release matrix tablets 羟丙基甲基纤维素的理化性质对富马酸喹硫平缓释基质片剂释放的影响
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-07 DOI: 10.1186/s13065-024-01311-2
Takwa E. Ellakwa, Ahmad S. Abu-Khadra, Doha El-Sayed Ellakwa

Quetiapine fumarateis a typical antipsychotic with a short half-life of 6 h and is administered multiple times daily. In this study, a copolymer for controlled delivery of quetiapine fumarate will be developed. In order to prevent side effects and improve patient compliance, hydroxypropyl methylcellulose K15M (HPMC K15M) was included in the formulation of the quetiapine fumarate oral sustained-release tablets at a concentration of 10–30%. A series of analytical methods were used to determine the characteristics of the prepared hydrogels, including Fourier transform-infrared spectroscopy, Differential scanning calorimetry, X-ray diffraction, and Scanning electron microscope. At two different pH values (1.2 and 6.8), swelling and release studies were conducted. A variety of release kinetic models was used to study drug release mechanisms. A non-Fickian diffusion mechanism released hydrogels prepared from quetiapine fumarate. It was found that swelling was increased by increasing the amount of HPMC K15M. Compared to the other batches (10–20%), the produced tablets with 30% HPMC K15M content had a better release profile after 20 h of dissolution. Because of the effective matrix complex’s limited solubility in water, the drug diffuses through the gel layer at a steady rate rather than dissolving quickly.

富马酸喹硫平是一种典型的抗精神病药物,半衰期短,仅为 6 小时,每天多次给药。本研究将开发一种用于控制富马酸喹硫平给药的共聚物。为了防止副作用并提高患者的依从性,羟丙基甲基纤维素 K15M(HPMC K15M)被添加到富马酸喹硫平口服缓释片的配方中,浓度为 10-30%。采用了一系列分析方法来确定所制备水凝胶的特性,包括傅立叶变换红外光谱法、差示扫描量热法、X射线衍射法和扫描电子显微镜。在两种不同的 pH 值(1.2 和 6.8)下,进行了溶胀和释放研究。研究人员使用了多种释放动力学模型来研究药物释放机制。富马酸喹硫平制备的水凝胶采用非菲克扩散机制释放药物。研究发现,增加 HPMC K15M 的用量可增加溶胀。与其他批次(10-20%)相比,HPMC K15M 含量为 30% 的片剂在溶解 20 小时后具有更好的释放曲线。由于有效基质复合物在水中的溶解度有限,药物以稳定的速度通过凝胶体层扩散,而不是快速溶解。
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引用次数: 0
La-supported SnO2–CaO composite catalysts for efficient malachite green degradation under UV–vis light 紫外可见光下用于高效降解孔雀石绿的 La-supported SnO2-CaO 复合催化剂
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-07 DOI: 10.1186/s13065-024-01332-x
Nastaran Parsafard, Ghazaleh Aghajari

This study presents the development and optimization of La@SnO2–CaO composite catalysts for efficient photocatalytic degradation of malachite green dye in aqueous solutions under UV–vis light irradiation. The catalysts were prepared via conventional incipient-wetness impregnation and thoroughly characterized using advanced analytical techniques, including X-ray diffraction, Fourier transform infrared spectroscopy, UV–vis diffuse reflectance spectroscopy, N2 adsorption–desorption analysis, and scanning electron microscopy. To optimize photodegradation efficiency, the effects of three independent factors were systematically investigated using response surface methodology: Temperature, pH, and Sn/Ca molar ratio. Our results reveal optimal conditions for maximum dye degradation: pH 7, Sn/Ca molar ratio of 0.33, and a process time of 35 min, resulting in a maximum photodegradation efficiency of 98.80% for malachite green dye. Notably, visible light exhibited a more pronounced effect on dye degradation compared to UV light over time, with visible light achieving 25% greater dye removal after 60 min of illumination. Furthermore, the catalyst showed excellent recyclability, retaining 85% of its initial activity after five consecutive cycles. These findings contribute significantly to the development of sustainable methods for dye removal from wastewater and highlight the potential of La@SnO2–CaO composite catalysts in environmental remediation processes, particularly in treating textile industry effluents.

本研究开发并优化了 La@SnO2-CaO 复合催化剂,用于在紫外-可见光照射下高效光催化降解水溶液中的孔雀石绿染料。催化剂的制备采用了传统的浸渍法,并利用先进的分析技术,包括 X 射线衍射、傅立叶变换红外光谱、紫外-可见光漫反射光谱、N2 吸附-解吸分析和扫描电子显微镜,对催化剂进行了全面表征。为了优化光降解效率,采用响应面方法系统地研究了三个独立因素的影响:温度、pH 值和 Sn/Ca 摩尔比。我们的研究结果表明了实现最大染料降解的最佳条件:pH 值为 7,锡/钙摩尔比为 0.33,处理时间为 35 分钟,从而使孔雀石绿染料的最大光降解效率达到 98.80%。值得注意的是,随着时间的推移,可见光对染料降解的影响比紫外线更明显,可见光照射 60 分钟后,染料去除率提高了 25%。此外,该催化剂还表现出极佳的可回收性,在连续使用五个周期后,其初始活性仍能保持 85%。这些发现极大地促进了可持续废水染料去除方法的开发,并凸显了 La@SnO2-CaO 复合催化剂在环境修复过程中的潜力,尤其是在处理纺织工业废水方面。
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引用次数: 0
Sustainable and efficient monitoring of tryptophan and tyrosine serum levels: a green HPTLC method as a biomarker for type 2 diabetes 可持续、高效地监测色氨酸和酪氨酸血清水平:作为 2 型糖尿病生物标志物的绿色 HPTLC 方法。
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-05 DOI: 10.1186/s13065-024-01318-9
Rania M. Kamel, Fatma A. M. Abdel-aal, Fardous A. Mohamed, Abdel-Maaboud I. Mohamed

In recent years, there has been considerable interest in using amino acids like tryptophan (Trp) and tyrosine (Tyr) as biomarkers for various diseases, including type 2 diabetes mellitus (T2D). In diseases like T2D, the metabolism of Trp and Tyr is altered. The activity of enzymes involved in Trp metabolism increases, leading to a decrease in its serum level. On the other hand, the serum level of Tyr increases due to the suppressed activity of its metabolizing enzymes. These observations suggest that Trp and Tyr metabolism may play a crucial role in the pathophysiology of type 2 diabetes. Our study highlights the potential utility of Trp and Tyr as biomarkers for the early detection, prognosis, and monitoring of this metabolic disorder. Given these observations, we aimed to develop a high-performance thin-layer chromatographic (HPTLC) method that is sensitive, selective, rapid, and environmentally friendly for estimating the concentrations of Trp and Tyr in biological fluids, particularly serum samples. To evaluate the method, we performed analysis using serum samples from controlled and streptozotocin-induced diabetic rats. Our main objective was to develop a method that is sensitive and selective for precisely determining Trp and Tyr serum levels, which could serve as potential biomarkers for T2D. Fluorescence and absorption modes were employed for densitometry scanning. We assessed the precision and high separation efficiency of the chromatographic system by calculating parameters such as separation and resolution factors, number of theoretical plates, and height equivalent to theoretical plates. To evaluate the environmental impact of our proposed method, we employed the AGREE (Analytical GREEnness metric) and GAPI (Green Analytical Procedure Index) greenness assessment tools. The results confirmed that our method is environmentally friendly and exhibits superior eco-friendliness and greenness compared to other reported methods.

Graphical Abstract

近年来,人们对使用色氨酸(Trp)和酪氨酸(Tyr)等氨基酸作为包括 2 型糖尿病(T2D)在内的各种疾病的生物标记物产生了浓厚的兴趣。在 2 型糖尿病等疾病中,Trp 和 Tyr 的代谢会发生改变。参与 Trp 代谢的酶的活性增加,导致其血清水平下降。另一方面,由于其代谢酶的活性受到抑制,血清中 Tyr 的水平会升高。这些观察结果表明,Trp 和 Tyr 的代谢可能在 2 型糖尿病的病理生理学中起着至关重要的作用。我们的研究强调了 Trp 和 Tyr 作为生物标记物在早期检测、预后和监测这种代谢紊乱方面的潜在作用。鉴于这些观察结果,我们旨在开发一种灵敏、选择性强、快速且环保的高效薄层色谱(HPTLC)方法,用于估算生物液体(尤其是血清样本)中 Trp 和 Tyr 的浓度。为了评估该方法,我们使用对照组和链脲佐菌素诱导的糖尿病大鼠的血清样本进行了分析。我们的主要目的是开发一种灵敏度高、选择性强的方法,用于精确测定血清中的 Trp 和 Tyr 水平,这两种物质可作为 T2D 的潜在生物标记物。采用荧光和吸收模式进行密度扫描。我们通过计算分离和分辨因子、理论板数和相当于理论板的高度等参数,评估了色谱系统的精确性和高分离效率。为了评估我们提出的方法对环境的影响,我们采用了 AGREE(分析环境优美度指标)和 GAPI(绿色分析程序指数)绿色评估工具。结果证实,我们的方法是环境友好型的,与其他已报道的方法相比,具有更优越的生态友好性和绿色性。
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引用次数: 0
Extraction of methamphetamine and pseudoephedrine by modified graphene oxide solid phase extraction method coupled to HPLC-UV in urine sample 尿样中甲基苯丙胺和伪麻黄碱的改良氧化石墨烯固相萃取-高效液相色谱-紫外检测法
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-05 DOI: 10.1186/s13065-024-01331-y
Nasim Nourani, Yousef Javadzadeh, Ali Shayanfar, Arezou Taghvimi, Ahad Bavili-Tabrizi, Siavoush Dastmalchi

Methamphetamine, pseudoephedrine, and related drugs are among the first drugs used for the stimulation of the central nervous system. In this study, two adsorbents based on graphene oxide (GO) were synthesized and used for the analysis of methamphetamine and pseudoephedrine. The prepared nano-adsorbents based on GO in this study were coated by polyaniline (PANI) and Fe3O4/C-nanodot/GO (magnetic adsorbent). The average size of nanoparticles (GO/PANI) was 18.43 nm. The specific surface area and pore size diameter of Fe3O4/C-nanodot/GO were 22.71 m2 g− 1 and 15.23 nm, respectively. Experimental variables affecting the extraction efficiency of the analytes such as pH of the sample solution, amount of adsorbent, extraction time, and type of eluents were investigated and optimized by response surface methodology. Under optimum conditions, GO/PANI and Fe3O4/C-nanodot/GO were considered appropriate solid phase extraction adsorbents for HPLC-based analyses of the studied drugs in human urine samples. However, GO/Fe3O4 nano adsorbent (Fe3O4/C-nanodot/GO) showed superior working condition than GO/PANI. The validated proposed analytical methods can be used for the quantitative determination of methamphetamine and pseudoephedrine in actual samples.

甲基苯丙胺、伪麻黄碱及相关药物是最早用于刺激中枢神经系统的药物之一。本研究合成了两种基于氧化石墨烯(GO)的吸附剂,并将其用于甲基苯丙胺和伪麻黄碱的分析。本研究中制备的基于 GO 的纳米吸附剂被聚苯胺(PANI)和 Fe3O4/C-nanodot/GO (磁性吸附剂)包覆。纳米颗粒(GO/PANI)的平均粒径为 18.43 nm。Fe3O4/C-nanodot/GO 的比表面积和孔径分别为 22.71 m2 g- 1 和 15.23 nm。采用响应面方法研究并优化了影响分析物萃取效率的实验变量,如样品溶液的 pH 值、吸附剂用量、萃取时间和洗脱液类型。在最佳条件下,GO/PANI 和 Fe3O4/C-nanodot/GO 被认为是基于 HPLC 分析人尿样中研究药物的合适固相萃取吸附剂。然而,GO/Fe3O4 纳米吸附剂(Fe3O4/C-nanodot/GO)的工作条件优于 GO/PANI。经过验证的拟议分析方法可用于实际样品中甲基苯丙胺和伪麻黄碱的定量检测。
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引用次数: 0
Development and validation of an LC‒MS/MS method for the determination of cyclocreatine phosphate and its related endogenous biomolecules in rat heart tissues 开发并验证测定大鼠心脏组织中环磷酸肌酸及其相关内源性生物大分子的 LC-MS/MS 方法。
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-04 DOI: 10.1186/s13065-024-01304-1
Ibrahim F. Abo-Elmagd, Amr M. Mahmoud, Medhat A. Al-Ghobashy, Marianne Nebsen, Mostafa A. Rabie, Ahmed F. Mohamed, Lamiaa A. Ahmed, Nesrine S. El Sayed, Reem K. Arafa, Robert Todd, Salwa A. Elgebaly

The cardioprotective drug cyclocreatine phosphate has been awarded Food and Drug Administration-orphan drug designation for the prevention of ischemic injury to enhance cardiac graft recovery and survival in heart transplantation. Cyclocreatine phosphate is the water-soluble derivative of cyclocreatine. Estimating the levels of Cyclocreatine phosphate, Adenosine triphosphate, Creatine Phosphate, Creatine and Cyclocreatine helps us in understanding the energy state as well as evaluating the heart cells’ function. The quantification of endogenous compounds imposes a challenging task for analysts because of the absence of a true blank matrix, whose use is required according to international guidelines. Recently, the International Council for Harmonization issued a new guideline that contains guidance on the validation of methods used to quantify endogenous components, such as the background subtraction approach that was employed in our current study. Specifically, we developed and validated a sensitive, reliable and accurate liquid chromatography-tandem mass spectrometry assay to determine simultaneously the levels of mentioned endogenous compounds in rat heart tissue. Tissue samples were prepared by protein precipitation extraction using water: methanol (1:1). Using Ultra Performance Liquid Chromatography, Chromatographic separation was achieved with ZORBAX Eclipse Plus C18 4.6 × 100 mm,3.5 μm column and conditions as following: ammonium acetate (pH 8.5): acetonitrile, 70:30 mobile phase, 0.7 mL/min flow rate and 25 °C temperature. Electrospray ionization mass detector with Multiple reaction monitoring mode was then employed, using both positive and negative modes, Analysis was carried out using 5.00–2000.00 ng/mL linear concentration range within 2 min for each analyte. According to Food and Drug Administration guidelines for bioanalytical methods, validation was carried out. We investigated the matrix effect, recovery efficiency and process efficiency for the analyte in neat solvent, postextraction matrix and tissue. The results stated mean percentage recoveries higher than 99%, accuracy 93.32–111.99%, and Relative Standard Deviation (RSD) below 15% within the concentration range of our study which indicated that target analytes’ stability in their real matrix is sufficient under the employed experimental conditions.

心脏保护药物磷酸环肌肽已被美国食品药品管理局认定为非专利药物,用于预防缺血性损伤,以提高心脏移植手术中的心脏移植物恢复和存活率。磷酸环肌酸是环肌酸的水溶性衍生物。估算磷酸环肌酸、三磷酸腺苷、磷酸肌酸、肌酸和环肌酸的水平有助于我们了解能量状态和评估心脏细胞的功能。由于缺乏真正的空白基质,内源性化合物的定量对分析人员来说是一项极具挑战性的任务。最近,国际协调理事会发布了一份新指南,其中包含对用于量化内源性成分的方法进行验证的指导,例如我们目前研究中采用的背景减去法。具体来说,我们开发并验证了一种灵敏、可靠、准确的液相色谱-串联质谱测定法,用于同时测定大鼠心脏组织中提及的内源性化合物的水平。组织样本采用水-甲醇(1:1)沉淀提取法制备。采用 ZORBAX Eclipse Plus C18 4.6 × 100 mm、3.5 μm 色谱柱,以乙酸铵(pH 8.5):乙腈(70:30)为流动相,流速 0.7 mL/min,柱温 25 ℃,进行超高效液相色谱分离。采用电喷雾离子化质量检测器和多反应监测模式,同时使用正离子和负离子模式,在 2 分钟内对每种分析物在 5.00-2000.00 纳克/毫升的线性浓度范围内进行分析。根据食品和药物管理局生物分析方法指南进行了验证。我们研究了分析物在纯溶剂、萃取后基质和组织中的基质效应、回收率和过程效率。结果表明,在我们研究的浓度范围内,平均回收率高于 99%,准确度为 93.32-111.99%,相对标准偏差(RSD)低于 15%。
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引用次数: 0
Measurement of tepotinib by UPLC‒MS/MS and its interaction with naringenin in rats 用 UPLC-MS/MS 测定大鼠体内的特博替尼及其与柚皮苷的相互作用。
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-04 DOI: 10.1186/s13065-024-01293-1
Zhe Chen, Chaojie Chen, Ya-nan Liu, Xinhao Xu, Shunbin Luo

We established a method based on ultra performance liquid chromatography tandem mass spectrometry (UPLC‒MS/MS) to quantitatively measure tepotinib, which was validated as acceptable and used in the evaluation of food-drug interactions between tepotinib and naringenin in rats. We used pemigatinib as the internal standard (IS), and acetonitrile and 0.1% formic acid aqueous solution constituted the mobile phase. To extract the target analyte, acetonitrile was used for protein precipitation (PPT). For UPLC‒MS/MS, we performed liquid chromatography using a C18 column, and mass spectrometry was performed in positive multiple reaction monitoring (MRM) mode. Excellent linearity was shown in the range of 0.1–500 ng/mL, and the coefficient of correlation was > 0.99. Notably, the lower limit of quantification (LLOQ) for tepotinib was determined to be 0.1 ng/mL. The intra- and inter-day accuracy of tepotinib ranged from − 1.7 to 7.3%, while the precision was ≤ 8.4%, at three concentrations except LLOQ. The recovery of each substance was ≥ 81.2%, and the matrix effects were within 90.5-98.6%. The stabilities of all analytes under different conditions met all requirements for quantitation in plasma samples. The relevant parameters, such as LLOQ, were evaluated in accordance with the principles of the Food and Drug Administration (FDA) biological verification method. Food-drug interaction study had shown that the plasma concentration of tepotinib could be significantly increased, accompanied by a decrease in clearance rate when administered with 50 mg/kg naringenin. The results showed that naringenin could increase the plasma concentration and decrease the clearance rate of tepotinib when naringenin and tepotinib were administered at the same time.

我们建立了一种基于超高效液相色谱-串联质谱(UPLC-MS/MS)的方法来定量测定特泊替尼,该方法经验证可用于特泊替尼和柚皮苷在大鼠体内的食物-药物相互作用评价。我们使用培美加替尼作为内标(IS),流动相为乙腈和 0.1% 甲酸水溶液。提取目标分析物时,使用乙腈进行蛋白质沉淀(PPT)。对于 UPLC-MS/MS,我们使用 C18 色谱柱进行液相色谱分析,并以正离子多反应监测(MRM)模式进行质谱分析。在 0.1-500 毫微克/毫升的范围内线性关系良好,相关系数大于 0.99。值得注意的是,特泊替尼的定量下限(LLOQ)被确定为 0.1 纳克/毫升。在除 LLOQ 以外的三个浓度下,特泊替尼的日内和日间准确度为 - 1.7% 至 7.3%,精密度≤ 8.4%。各物质的回收率均≥81.2%,基质效应在90.5%-98.6%之间。所有分析物在不同条件下的稳定性均满足血浆样品定量的所有要求。LLOQ等相关参数的评估符合美国食品药品管理局(FDA)生物验证方法的原则。食物与药物相互作用研究表明,与 50 mg/kg 柚皮甙同时服用时,特泊替尼的血浆浓度会显著升高,同时清除率降低。结果表明,同时服用柚皮苷和特泊替尼时,柚皮苷可增加特泊替尼的血浆浓度并降低其清除率。
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引用次数: 0
Bioassay-guided isolation and in Silico characterization of cytotoxic compounds from Hemimycale sp. Sponge targeting A549 lung cancer cells 生物测定指导下从 Hemimycale sp.海绵中针对 A549 肺癌细胞的细胞毒性化合物的分离和硅学表征。
IF 4.3 2区 化学 Q2 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-01 DOI: 10.1186/s13065-024-01325-w
Asmaa Abo Elgoud Said, Islam M. Abdel-Rahman, Yaser A. Mostafa, Eman Zekry Attia, Mamdouh Nabil Samy, Usama Ramadan Abdelmohsen, Katsuyoshi Matsunami, Mostafa A. Fouad, Yaser G. Gouda

Bioassay-guided fractionation approach led to identification of two novel compounds; (4-(hydroxymethyl)-3-methoxy-1H-pyrazol (1) and mycalene (2), alongside with four known metabolites; octadecane (3), hexatriacontane (4), 1-heneicosanol (5) and heptatriacontanoic acid (6) from the Red Sea marine sponge Hemimycale sp. The ethyl acetate fraction showed a noticeable cytotoxic activity against the lung cancer cell line (A549) with IC50 value of 75.54 µg/ mL. Structural elucidation was achieved using a combination of 1D and 2D nuclear magnetic resonance (NMR) spectroscopy and high-resolution electrospray ionization-mass spectrometry (HR-ESI-MS). To elucidate the potential mechanism of action behind the cytotoxic effects against lung cancer, a multi-faceted approach combining in silico network pharmacology, experimental validation, and molecular docking studies were employed. Both compounds, designated as 1 and 2, demonstrated significant binding affinities to predicted target proteins, with docking scores of -4.789 and − 4.421 kcal/mol, respectively. These results lay the groundwork for further investigation into the therapeutic potential of these novel compounds from Hemimycale sp. as promising candidates for lung cancer treatment.

通过生物测定指导下的分馏方法,从红海海洋海绵 Hemimycale sp.中鉴定出了两种新型化合物:4-(羟甲基)-3-甲氧基-1H-吡唑(1)和霉菌醛(2),以及四种已知代谢物:十八烷(3)、十六烷(4)、1-heneicosanol(5)和七烷酸(6)。乙酸乙酯馏分对肺癌细胞株(A549)具有明显的细胞毒性活性,IC50 值为 75.54 µg/ mL。利用一维和二维核磁共振(NMR)光谱以及高分辨率电喷雾电离质谱(HR-ESI-MS)相结合的方法对其结构进行了阐明。为了阐明肺癌细胞毒性作用背后的潜在作用机制,研究人员采用了一种结合了硅网络药理学、实验验证和分子对接研究的多元方法。这两种化合物(分别命名为 1 和 2)与预测的靶蛋白具有显著的结合亲和力,对接得分分别为 -4.789 和 - 4.421 kcal/mol。这些结果为进一步研究这些来自血鳞藻类的新型化合物的治疗潜力奠定了基础,它们有望成为肺癌治疗的候选化合物。
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引用次数: 0
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