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Study on the Spectrum-Effect Correlation of Anti-Inflammatory Active Extract of Sauropus spatulifolius Beille 小檗抗炎活性提取物的光谱效应相关性研究
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-05-24 DOI: 10.1155/2022/5646546
Q. Qiu, L. Jiang, Chunying Huang, Lifeng Yu, Dandan Zhen, M. Ye, Yuanyuan Liu, Ju-hong Shi, Xiaofang Liu, Baojun Gu, H. Zhen
Sauropus spatulifolius Beille (S. spatulifolius) is a commonly used medicine of the Bourau and Yao nationalities. However, the composition of S. spatulifolius is complex, and simple chemical fingerprints cannot accurately evaluate the relationship between its composition and efficacy. In this study, high-performance liquid chromatography (HPLC) method was used to establish the fingerprint of the ethyl acetate extract of S. spatulifolius. Based on the evaluation of the similarity of chromatographic fingerprints of traditional Chinese medicine, combined with cluster analysis and principal component analysis (PCA), the common peaks of fingerprints were evaluated. The anti-inflammatory effect data were extracted through the dimethylbenzene-induced ear-swelling model in mice. The gray relational analysis (GRA) combined with partial least squares regression (PLSR) was used to study the spectrum-effect correlation of S. spatulifolius. As a result, the HPLC fingerprint of the ethyl acetate extract of S. spatulifolius was established, and 18 common peaks were identified. Except for S6, the other similarities are all above 0.915. The reference substance control method was used to identify two absorption peaks, namely, protocatechuic acid and caffeic acid. The cluster analysis results showed that 10 samples from different origins were grouped into four categories, which was consistent with the PCA results. Ethyl acetate extract of 10 batches of S. spatulifolius could significantly inhibit the ear swelling of mice (P < 0.01). Through GRA, the order of the contribution of each chemical component to the anti-inflammatory efficacy was obtained. The results of PLSR showed that the VIP values of peaks 3, 4, and 12 were greater than 1 and were positively correlated with anti-inflammatory activity. In this study, the HPLC fingerprint of the ethyl acetate extract of S. spatulifolius was established. Through the study of the spectrum-effect correlation, the anti-inflammatory active substance of the ethyl acetate extract of S. spatulifolius was obtained. The anti-inflammatory effect of S. spatulifolius was the result of the joint action of multiple ingredients. This research helps to quickly and accurately discover the active ingredient groups of traditional Chinese medicine and provides new ideas and methods for studying the effective substances of traditional Chinese medicine.
小刀龙(Sauropus spatulifolius Beille)是瑶族、瑶族的常用药材。然而,小檗的成分复杂,简单的化学指纹图谱无法准确评价其成分与药效的关系。本研究采用高效液相色谱法(HPLC)建立了鸡血藤乙酸乙酯提取物的指纹图谱。在评价中药色谱指纹图谱相似度的基础上,结合聚类分析和主成分分析(PCA)对指纹图谱的共同峰进行了评价。通过二甲基苯致小鼠耳肿胀模型提取抗炎作用数据。采用灰色关联分析(GRA)和偏最小二乘回归(PLSR)相结合的方法,研究了小黄菜的光谱效应相关性。建立了小檗乙酸乙酯提取物的HPLC指纹图谱,鉴定出18个共有峰。除S6外,其他相似度均在0.915以上。采用标准物质对照法鉴定了原儿茶酸和咖啡酸两个吸收峰。聚类分析结果显示,来自不同产地的10个样品被归为4类,这与主成分分析结果一致。10批小檗乙酸乙酯提取物对小鼠耳肿胀有显著抑制作用(P < 0.01)。通过GRA,得到各化学成分对抗炎功效的贡献顺序。PLSR结果显示,峰3、峰4、峰12的VIP值均大于1,与抗炎活性呈正相关。本研究建立了小檗乙酸乙酯提取物的HPLC指纹图谱。通过光谱效应相关性研究,得到了小檗乙酸乙酯提取物的抗炎活性物质。小檗的抗炎作用是多种成分共同作用的结果。本研究有助于快速准确地发现中药有效成分群,为研究中药有效物质提供了新的思路和方法。
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引用次数: 3
Current-Volt Biosensing “Cystatin C” on Carbon Nanowired Interdigitated Electrode Surface: A Clinical Marker Analysis for Bulged Aorta 碳纳米线交叉指状电极表面的电流-伏特生物传感“胱抑素C”:主动脉肿胀的临床标志物分析
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-05-23 DOI: 10.1155/2022/8160502
X. Chen, Jie Kang, Qiu Sun, Cheng Liu, Hongling Wang, Chen Wang, S. Gopinath
A carbon nanowire-modified surface with interdigitated electrode (IDE) sensing system was introduced to identify abdominal aortic aneurysm biomarker “papain,” also known as cysteine protease, used as the capture probe to identify Cystatin C. Papain was immobilized through the covalent integration of amine group on papain and the carboxyl group with carbon nanowire. This papain-modified electrode surface was utilized to detect the different concentrations of Cystatin C (100 pg/mL to 3.2 ng/mL). The interaction between papain and Cystatin C was monitored using a picoammeter, and the response curves were compared. With increasing Cystatin C concentrations, the total current levels were gradually increased with a linear range from 200 pg/mL to 3.2 ng/mL, and the current differences were plotted and the detection limit of Cystatin C was calculated as 200 pg/mL. The averaging of three independent experiments (n = 3) was made with 3δ estimation, and the determination coefficient was y = 1.8477 × 0.7303 and R2 = 0.9878. Furthermore, control experiments with creatinine and gliadin failed to bind the immobilized papain, indicating the specific detection of Cystatin C.
采用碳纳米线修饰表面与交叉指状电极(IDE)传感系统来识别腹主动脉瘤生物标志物“木瓜蛋白酶”,也称为半胱氨酸蛋白酶,并将其作为捕获探针来识别胱抑素c。木瓜蛋白酶通过在木瓜蛋白酶上的胺基与羧基与碳纳米线的共价整合来固定。利用木瓜蛋白酶修饰的电极表面检测不同浓度的胱抑素C (100 pg/mL至3.2 ng/mL)。用皮安计监测木瓜蛋白酶与胱抑素C的相互作用,比较反应曲线。随着Cystatin C浓度的增加,总电流水平在200 pg/mL ~ 3.2 ng/mL的线性范围内逐渐增加,绘制电流差值图,计算Cystatin C的检出限为200 pg/mL。对3个独立实验(n = 3)取平均值,采用3δ估计,决定系数为y = 1.8477 × 0.7303, R2 = 0.9878。此外,肌酐和麦胶蛋白的对照实验未能结合固定化的木瓜蛋白酶,这表明胱抑素C的特异性检测。
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引用次数: 0
Study of Saponin Components after Biotransformation of Dioscorea nipponica by Endophytic Fungi C39 内生真菌C39对薯蓣生物转化后皂苷成分的研究
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-05-11 DOI: 10.1155/2022/2943177
Nannan Huang, Dan Yu, J. Huo, Junkai Wu, Yiyang Chen, Xiaowei Du, Xi-jun Wang
This study conducted the solid fermentation process of Dioscorea nipponica using endophytic fungi C39 to determine the changes in the diosgenin concentration. The results revealed that endophytic fungi C39 could effectively biotransform the saponin components in D. nipponica. Moreover, the maximum increase in the diosgenin concentration reached 62.67% in 15 days of solid fermentation. MTT assay results demonstrated that the inhibitory effects of the fermentation drugs on four types of cancer cells (liver cancer cells (HepG2), stomach cancer cells (BGC823), cervical cancer cells (HeLa), and lung cancer cells (A549)) were better than those of the crude drugs obtained from D. nipponica. The chemical composition of the samples obtained before and after the biotransformation of D. nipponica was analyzed by UPLC-Q-TOF-MS. A total of 32 compounds were identified, 21 of which have been reported in Dioscorea saponins and the ChemSpider database and 11 compounds were identified for the first time in D. nipponica. The biotransformation process was inferred based on the variation trend of saponins, which included transformation pathways pertaining to glycolytic metabolism, ring closure reaction, dehydrogenation, and carbonylation. The cumulative findings provide the basis for the rapid qualitative analysis of the saponin components of D. nipponica before and after biotransformation. The 11 metabolites obtained from biotransformation are potential active ingredients obtained from D. nipponica, which can be used to further identify pharmacodynamically active substances.
本研究利用内生真菌C39对日本薯蓣进行固体发酵过程,测定薯蓣皂苷元浓度的变化。结果表明,内生真菌C39能有效地转化日本龙葵中的皂苷成分。固体发酵15 d时,薯蓣皂苷元浓度增幅最大,达62.67%。MTT实验结果表明,发酵药物对肝癌细胞(HepG2)、胃癌细胞(BGC823)、宫颈癌细胞(HeLa)和肺癌细胞(A549)的抑制作用优于日本菜生药。采用UPLC-Q-TOF-MS对日本龙葵生物转化前后样品的化学成分进行分析。共鉴定出32个化合物,其中21个为首次从薯蓣皂苷中分离得到,11个为首次从薯蓣皂苷中分离得到。根据皂苷的变化趋势推断其生物转化过程包括糖酵解代谢、环闭合反应、脱氢和羰基化等转化途径。这些累积结果为快速定性分析龙葵生物转化前后的皂苷成分提供了依据。通过生物转化得到的11种代谢物均为日本龙葵中潜在的活性成分,可用于进一步鉴定药效学活性物质。
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引用次数: 2
Carbon Material Hybrid Construction on an Aptasensor for Monitoring Surgical Tumors 用于外科肿瘤监测的碳材料复合传感器
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-05-10 DOI: 10.1155/2022/9740784
Renyuan Ma, Subash C. B. Gopinath, T. LakshmiPriya, Yeng Chen
Carcinoembryonic antigen (CEA) is a glycoprotein, one of the common tumor biomarkers, found at low levels in body fluids. Generally, overexpression of CEA is found in various cancers, including ovarian, breast, lung, colorectal, gastric, and pancreatic cancers. Since CEA is an important tumor biomarker, the quantification of CEA is helpful for diagnosing cancer, monitoring tumor progression, and the follow-up treatment. This research develops a highly sensitive sandwich aptasensor for CEA identification on an interdigitated electrode sensor. Carbon-based material was used to attach a higher anti-CEA capture aptamer onto the sensor surface through a chemical linker, and then, CEA was quantified by the aptamer. Furthermore, CEA-spiked serum was tested by using the immobilized aptamer, which was found to not affect the target validation. The limit of detection for CEA in PBS and serum is calculated from a linear regression graph to be 0.5 ng/mL with R2 values of 0.9593 and 0.9657, respectively, over a linear range from 0.5 to 500 ng/mL. This CEA quantification by the aptasensor can help diagnose various surgical tumors and monitor their progression.
癌胚抗原(CEA)是一种糖蛋白,是常见的肿瘤生物标志物之一,在体液中含量较低。通常,CEA过表达存在于多种癌症中,包括卵巢癌、乳腺癌、肺癌、结直肠癌、胃癌和胰腺癌。由于CEA是一种重要的肿瘤生物标志物,因此CEA的量化有助于癌症的诊断、肿瘤进展的监测和后续治疗。本研究在交叉指状电极传感器上开发了一种高灵敏度的CEA夹芯感应传感器。利用碳基材料通过化学连接剂将较高的抗CEA捕获适体附着在传感器表面,然后通过适体对CEA进行量化。此外,用固定化适体检测cea加标血清,发现其不影响靶标验证。在0.5 ~ 500 ng/mL的线性范围内,通过线性回归图计算出PBS和血清中CEA的检出限为0.5 ng/mL, R2分别为0.9593和0.9657。通过配体传感器对CEA进行量化可以帮助诊断各种外科肿瘤并监测其进展。
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引用次数: 4
Detection of Falsified Antimalarial Sulfadoxine-Pyrimethamine and Dihydroartemisinin-Piperaquine Drugs Using a Low-Cost Handheld Near-Infrared Spectrometer 低成本手持式近红外光谱仪检测伪造抗疟药物磺胺多辛-乙胺嘧啶和双氢青蒿素-哌喹
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-05-03 DOI: 10.1155/2022/5335936
Moussa Yabré, A. K. Sakira, M. Bandé, Bertrand W. F. Goumbri, S. M. Ouattara, S. Fofana, T. I. Somé
Falsified drugs are of serious concern to public health worldwide, particularly for developing countries where quality control of drugs is inefficient. In law enforcement against such fake medicines, there is a need to develop reliable, fast, and inexpensive screening methods. In this work, the ability of an innovative low-cost handheld near-infrared spectrometer to identify falsifications among two antimalarial fixed dose combination tablets, dihydroartemisinin/piperaquine and sulfadoxine/pyrimethamine, has been investigated. Analyzed samples were collected in Burkina Faso mainly in rural transborder areas that could be infiltrated by illicit drugs. A principal component analysis was applied on the acquired near-infrared spectra to identify trends, similarities, and differences between collected samples. This allowed to detect some samples of dihydroartemisinin/piperaquine and sulfadoxine/pyrimethamine which seemed to be falsified. These suspicious samples were semiquantitatively analyzed by thin-layer chromatography using Minalab® kits. Obtained results allowed to confirm the falsifications since the suspected samples did not contain any of the expected active pharmaceutical ingredients. The capacity of the low-cost near-infrared device to identify specifically a brand name of dihydroartemisinin/piperaquine or sulfadoxine/pyrimethamine has been also studied using soft independent modelling of class analogy (SIMCA) in the classical and data driven versions. The built models allowed a clear brand identification with 100% of both sensitivity and specificity in the studied cases. All these results demonstrate the potential of these low-cost near-infrared spectrometers to be used as first line screening tools, particularly in resource limited laboratories, for the detection of falsified antimalarial drugs.
假药是全世界公共卫生的一个严重问题,特别是对药品质量控制效率低下的发展中国家。在打击此类假药的执法中,有必要开发可靠、快速和廉价的筛查方法。在这项工作中,研究了一种创新的低成本手持式近红外光谱仪识别两种抗疟疾固定剂量复方片剂(双氢青蒿素/哌喹和磺胺多辛/乙胺嘧啶)的伪造能力。分析的样本主要是在布基纳法索的农村跨境地区收集的,这些地区可能被非法药物渗透。主成分分析应用于获取的近红外光谱,以确定所收集样品之间的趋势,相似点和差异。这使得检测到一些似乎是伪造的双氢青蒿素/哌喹和磺胺多辛/乙胺嘧啶样品成为可能。使用Minalab®试剂盒对可疑样品进行薄层色谱半定量分析。所获得的结果允许确认伪造,因为可疑样品不含任何预期的有效药物成分。在经典版本和数据驱动版本中,还使用类类比的软独立建模(SIMCA)研究了低成本近红外设备识别双氢青蒿素/哌喹或磺胺多辛/乙胺嘧啶品牌名称的能力。在所研究的案例中,所建立的模型能够以100%的灵敏度和特异性清晰地识别品牌。所有这些结果表明,这些低成本近红外光谱仪有潜力用作一线筛选工具,特别是在资源有限的实验室中,用于检测伪造的抗疟药物。
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引用次数: 2
Erythrocyte Storage Lesion Improvements Mediated by Naringin Screened from Vegetable/Fruit Juice Using Cell Extract and HPLC-MS 利用细胞提取物和高效液相色谱-质谱联用技术从蔬菜/果汁中筛选柚皮苷改善红细胞储存损伤
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-04-26 DOI: 10.1155/2022/7556219
Yuqi She, Qiong Liu, Xiyue Xiong, Ning Li, Jian Zhang
In blood banking, storage at 4°C for weeks is known to cause damages to erythrocytes, called storage lesions that may later cause transfusion-related adverse events. In previous experiments, we found that vegetable/fruit juices can effectively reduce the storage lesion. Currently, we attempt to analyze the potential bioactive components and test whether the compounds can improve the storage lesions of erythrocytes. Equal portions in wet weight of 20 fresh vegetables and fruits were blended with phosphate buffered solution (PBS), and clear solutions were produced as additive to the packed erythrocytes from consented blood donors at 1 : 10 ratio (ml : gram). The blood samples were stored for 35 days at 4°C, and the supernatants were performed high liquid chromatography–mass spectrometry (HPLC-MS) analysis at 0 days, 14 days, and 35 days. The blood bags supplemented with identified bioactive components were stored in a refrigerator for 35 days, and the morphology, complete blood count (CBC), phosphatidylserine (PS) extroversion, hemolysis, and reactive oxygen species (ROS) levels were measured at the end of storage. Five potential bioactive components from vegetable/fruit juices contributed to the improvements of storage lesion. One of the compounds was unequivocally identified as naringin, and two were tentatively assigned as vitexin 6″-O-malonyl 2″-O-xyloside and luteolin 7-(6″-malonyl neohesperidoside). Naringin alleviated the storage lesion of red blood cells (RBCs) by reducing ROS levels and living cell extraction with HPLC-MS is a simple, reliable, and effective method for screening potential bioactive components.
在血库中,在4°C下储存数周已知会对红细胞造成损害,称为储存损伤,随后可能引起与输血相关的不良事件。在之前的实验中,我们发现蔬菜/果汁可以有效地减少贮藏损伤。目前,我们试图分析潜在的生物活性成分,并测试这些化合物是否能改善红细胞的储存病变。将20种新鲜蔬菜和水果按湿重等份与磷酸盐缓冲溶液(PBS)混合,制成透明溶液,以1:10的比例(ml: g)添加到经同意的献血者的红细胞中。血样在4℃下保存35 d,上清液在第0天、第14天和第35天进行高效液相色谱-质谱(HPLC-MS)分析。添加鉴定生物活性成分的血袋在冰箱中保存35 d,保存结束时检测形态学、全血细胞计数(CBC)、磷脂酰丝氨酸(PS)外移、溶血和活性氧(ROS)水平。果蔬汁中5种潜在的生物活性成分有助于改善贮藏损伤。其中一种化合物被明确鉴定为柚皮苷,另外两种化合物被初步鉴定为牡荆素6″- o -丙二烯基2″- o -木糖苷和木犀草素7-(6″-丙二烯基新橙皮苷)。柚皮苷通过降低活性氧(ROS)水平减轻红细胞贮藏损伤,高效液相色谱-质谱法提取活细胞是一种简单、可靠、有效的筛选潜在生物活性成分的方法。
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引用次数: 1
Photoreduction of CO2 to CH4 over Efficient Z-Scheme γ-Fe2O3/g-C3N4 Composites 高效Z-Scheme γ-Fe2O3/g-C3N4复合材料上CO2光还原成CH4的研究
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-04-26 DOI: 10.1155/2022/1358437
Thanh-Binh Nguyen, Thuy Hang Dinh Thi, D. Pham Minh, Hien Bui Minh, Ngoc Quynh Nguyen Thi, Bang Nguyen Dinh
A series of composite γ-Fe2O3/g-C3N4 (denoted as xFeCN with x equal 5, 10, 15, and 20 of γ-Fe2O3 percentage in weight) was prepared by calcination and precipitation-impregnation methods. X-ray diffraction (XRD), Fourier transform infrared (FTIR), and X-ray photoelectron spectrometry (XPS) characterizations indicated the successful synthesis of Z-scheme FeCN composites. A red shift of the light absorption region was revealed by UV-vis diffuse reflectance spectroscopy (UV-DRS). In addition, photoluminescence spectroscopy (PL) spectra showed an interface interaction of two phases Fe2O3 and g-C3N4 in the synthesized composites that improved the charge transfer capacity. The photocatalytic activity of these materials was studied in the photoreduction of CO2 with H2O as the reductant in the gaseous phase. The composites exhibited excellent photoactivity compared to undoped g-C3N4. The CH4 production rate over 10FeCN and 15FeCN composites (2.8 × 10−2 and 2.9 × 10−2 μmol h−1 g−1, respectively) was ca. 7 times higher than that over pristine g-C3N4 (0.4 × 10−2 μmol h−1 g−1). This outstanding photocatalytic property of these composites was explained by the light absorption expansion and the prevention of photogenerated electron-hole pairs recombination due to its Z-scheme structure.
采用煅烧和沉淀浸渍法制备了一系列γ-Fe2O3/g-C3N4复合材料(记为xFeCN, x分别为γ-Fe2O3的5、10、15和20)。x射线衍射(XRD)、傅立叶变换红外(FTIR)和x射线光电子能谱(XPS)表征表明Z-scheme FeCN复合材料的成功合成。紫外-可见漫反射光谱(UV-DRS)显示了光吸收区的红移。此外,光致发光光谱(PL)表明,合成的复合材料中存在Fe2O3和g-C3N4两相的界面相互作用,提高了电荷转移能力。研究了这些材料在气相以H2O为还原剂光还原CO2时的光催化活性。与未掺杂的g-C3N4相比,复合材料具有优异的光活性。10FeCN和15FeCN复合材料(分别为2.8 × 10−2和2.9 × 10−2 μmol h−1 g−1)的CH4产率比原始g- c3n4 (0.4 × 10−2 μmol h−1 g−1)的CH4产率高约7倍。这些复合材料具有优异的光催化性能,其原因是由于其z型结构的光吸收扩展和防止光生电子-空穴对复合。
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引用次数: 3
The Alkaline Resistance of Waterborne Acrylic Polymer/SiO2 Nanocomposite Coatings 水性丙烯酸聚合物/SiO2纳米复合涂料的耐碱性研究
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-04-22 DOI: 10.1155/2022/8266576
H. Thuy, H. Ha, Nguyen Thien Vuong, Tuan Anh Nguyen
This study presents a study on the influence of nano-SiO2 on the alkaline resistance of waterborne acrylic coating using some analysis methods such as FT-IR and UV-Vis spectroscopy, combined with FE-SEM analysis and monitoring weight and adhesion changes during exposure to the saturated Ca(OH)2 alkaline environment. The obtained results indicated that the alkaline resistance of acrylic coating enhanced appreciably when adding 2.5 wt% of nano-SiO2. Under the impact of the saturated Ca(OH)2 solution for 20 days of immersion, nanocomposite coating containing 2.5 wt.% of nano-SiO2 was only decreased by 3.6% of the weight and 15.4% of the adhesion, while the neat acrylic coating (without nano-SiO2) seriously reduced 25.4% of the weight and 39.1% of the adhesion.
本研究采用FT-IR、UV-Vis光谱等分析方法,结合FE-SEM分析,并监测饱和Ca(OH)2碱性环境下,纳米sio2对水性丙烯酸涂料耐碱性的影响。结果表明,当纳米sio2含量为2.5 wt%时,丙烯酸涂料的耐碱性明显增强。在饱和Ca(OH)2溶液浸泡20天的影响下,纳米复合涂层含2.5 wt。纳米sio2的掺入仅使涂层重量降低3.6%,附着力降低15.4%,而未掺入纳米sio2的纯丙烯酸涂层则使涂层重量降低25.4%,附着力降低39.1%。
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引用次数: 0
Development and Validation of a Liquid Chromatography-Mass Spectrometry Assay for Determination of Cromolyn Sodium in Skin Permeation Studies 液相色谱-质谱联用法测定皮肤渗透研究中色氨酸钠含量的建立与验证
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-04-21 DOI: 10.1155/2022/7437905
M. Holman, Stacy D. Brown, Dorcas Frempong, A. Puri, S. Dinh
Cromolyn sodium (CS) is a mast cell stabilizer administered to treat allergic diseases. A topical system would sustain its delivery and may be designed for treatment of atopic dermatitis. Established HPLC protocols for detection of CS are time consuming and intensive, indicating the need for a more streamlined method. This study aimed at developing and validating a sensitive and selective LC-MS method for quantifying CS in skin permeation studies that was less time and resource demanding. The optimized method involved an isocratic mobile phase (10 mM NH4HCO3, pH 8.0, 90% and ACN, 10%) at a flow rate of 0.25 mL/min. Detection involved direct MS/MS channels with m/z 467.0255 (precursor) and m/z 379.0517 (fragment) using argon as the collision gas. CS calibrants were prepared in PBS, pH 7.4, and methanol for validation (0.1–2.5 μg/mL). To ensure no skin interference, dermatomed porcine skin was mounted on Franz diffusion cells that were analyzed after 24 h. The skin layers were also separated, extracted in methanol, and analyzed using the developed method. Retention time was 1.9 min and 4.1 min in methanol and buffer, respectively. No interfering peaks were observed from the receptor and skin extracts, and linearity was established between 0.1 and 2.5 μg/mL. Interday and intraday accuracy and precision were within the acceptable limit of ±20% at the LLOQ and ±15% at other concentrations. Overall, the simplified, validated method showed sensitivity in detecting CS in skin without interference and was applied to demonstrate quantification of drug in skin following 4% cromolyn sodium gel exposure.
色胺酸钠(CS)是一种肥大细胞稳定剂,用于治疗过敏性疾病。局部系统将维持其递送,并可设计用于治疗特应性皮炎。建立的高效液相色谱检测CS的方案耗时且密集,表明需要更精简的方法。本研究旨在开发和验证一种敏感和选择性的LC-MS方法,用于在皮肤渗透研究中定量CS,减少时间和资源需求。优化后的方法采用等容流动相(10 mM NH4HCO3, pH 8.0, 90%, ACN, 10%),流速为0.25 mL/min。用氩作为碰撞气体,用m/z 467.0255(前驱体)和m/z 379.0517(碎片)进行直接质谱通道检测。CS校准剂分别在PBS、pH 7.4和甲醇中制备(0.1-2.5 μg/mL)进行验证。为确保无皮肤干扰,将剥去皮的猪皮置于Franz扩散池上,24 h后进行分析。皮肤层也被分离,在甲醇中提取,并使用所开发的方法分析。在甲醇和缓冲液中的保留时间分别为1.9 min和4.1 min。受体和皮肤提取物均未见干扰峰,在0.1 ~ 2.5 μg/mL范围内建立线性关系。日内和日间的准确度和精密度在最低限±20%和其他浓度±15%的可接受限度内。总的来说,简化的、经过验证的方法在无干扰的情况下检测皮肤中的CS具有敏感性,并应用于4%色胺酸钠凝胶暴露后皮肤中药物的定量。
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引用次数: 0
Enhanced Electrochemical Sensor for Electrocatalytic Glucose Analysis in Orange Juices and Milk by the Integration of the Electron-Withdrawing Substituents on Graphene/Glassy Carbon Electrode 石墨烯/玻璃碳电极上吸电子取代基集成用于橙汁和牛奶中葡萄糖电催化分析的增强型电化学传感器
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-04-12 DOI: 10.1155/2022/5029036
R. Zainul, I. Isa, Siti Nur Akmar Mohd Yazid, N. Hashim, Sharifah Norain Mohd Sharif, M. I. Saidin, M. S. Ahmad, M.Si Suyanta, Yulkifli Amir
In this work, a novel electrochemical sensor was developed by electron-withdrawing substituent modification of 1-phenyl-3-methyl-4-(4-fluorobenzoyl)-5-pyrazolone on a graphene-modified glassy carbon electrode (HPMpFP-graphene/GCE) for glucose detection. The results of characterizations using a scanning electron microscope, Fourier transform infrared spectroscopy, Raman spectroscopy, and nuclear magnetic resonance spectroscopy showed the successful fabrication of HPMpFP-graphene nanocomposite, which served as an electroactive probe for glucose detection. The electron transfer ability of HPMpFBP-graphene/GCE has been successfully revealed using cyclic voltammetry and electrochemical impedance spectroscopy results. The good electrochemical performance was shown by well-defined peak currents of square wave voltammetry under various parameters, including pH, HPMpFP and graphene composition, and scan rate effect. A high electrochemically evaluated surface area using chronoamperometry suggested that the present glucose detection response was intensified. The chronoamperometry results at a work potential of 0.4 V presented a wide linear range of 1 × 103–90 µM and 88–1 µM with 0.74 µM (S/N = 3) as the detection limit. An acceptable recovery has been revealed in the real sample analysis. The electrochemical sensing behaviour of the composite indicates that it may be a promising candidate for a glucose sensor and it significantly extends the range of applications in the electrochemical field.
在这项工作中,通过在石墨烯修饰的玻璃碳电极(hmpfp -graphene/GCE)上对1-苯基-3-甲基-4-(4-氟苯甲酰)-5-吡唑酮进行吸电子取代基修饰,开发了一种用于葡萄糖检测的新型电化学传感器。利用扫描电镜、傅里叶变换红外光谱、拉曼光谱和核磁共振光谱对其进行表征,结果表明hmpfp -石墨烯纳米复合材料的制备成功,可作为葡萄糖检测的电活性探针。hmpfbp -石墨烯/GCE的电子转移能力已通过循环伏安法和电化学阻抗谱分析成功揭示。在pH、HPMpFP、石墨烯成分等不同参数下,方波伏安峰值电流分布清晰,扫描速率效应明显,显示出良好的电化学性能。高电化学评价表面积使用时安培法表明,目前的葡萄糖检测响应加强。工作电位为0.4 V时,计时电流测量结果线性范围为1 × 103 ~ 90µM和88 ~ 1µM,检出限为0.74µM (S/N = 3)。在实际样品分析中显示出可接受的回收率。该复合材料的电化学传感性能表明,它可能是一个有前途的葡萄糖传感器的候选者,它大大扩展了电化学领域的应用范围。
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引用次数: 2
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Journal of Analytical Methods in Chemistry
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