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Development and Validation of UV Spectrophotometric Method for Determination of Prazosin Hydrochloride 用于测定盐酸哌唑嗪的紫外分光光度法的开发与验证
IF 0.8 4区 化学 Q4 SPECTROSCOPY Pub Date : 2024-07-04 DOI: 10.1007/s10812-024-01771-3
Chodimella Sahitya Bharathi, Raja Sundararajan

This work was aimed at creating a new, fast, and accurate UV spectrophotometric method for quantifying prazosin hydrochloride in pure and tablet dosage forms. A phosphate buffer solution of pH 6 was used as a diluent. The highest absorbance of prazosin hydrochloride was measured at 247 nm, and the linearity ranged from 2 to 8 μg/mL. The regression equation for prazosin hydrochloride was y= 0.087x + 0.236, with a correlation value 0.987. The percentage of recovery ranged from 99.6 to 101%. The relative standard deviation for intraday precision and interday precision was determined to be less than 2. The LOD and LOQ of prazosin hydrochloride were determined to be 0.0375 and 0.113 μg/mL, respectively. International Council for Harmonisation criteria validated the spectrometric technique and was suitable for routine quantitative measurement of prazosin hydrochloride in pure and tablet dosage forms.

本研究旨在建立一种新型、快速、准确的紫外分光光度法,用于定量检测纯品和片剂中的盐酸哌唑嗪。采用 pH 值为 6 的磷酸盐缓冲溶液作为稀释剂。盐酸哌唑嗪的最高吸光度为 247 nm,线性范围为 2 至 8 μg/mL。盐酸哌唑嗪的回归方程为 y= 0.087x + 0.236,相关系数为 0.987。回收率为 99.6%至 101%。日内精密度和日间精密度的相对标准偏差均小于 2。盐酸哌唑嗪的最低检测限和最低定量限分别为 0.0375 和 0.113 μg/mL。国际协调委员会的标准验证了该光谱分析技术,适用于纯品和片剂盐酸哌唑嗪的常规定量测定。
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引用次数: 0
Derivative Spectrophotometric Methods for Determination of Idelalisib in Bulk and in Formulation 测定散装和制剂中伊德拉利西的衍生分光光度法
IF 0.8 4区 化学 Q4 SPECTROSCOPY Pub Date : 2024-07-04 DOI: 10.1007/s10812-024-01772-2
Marella Mahesh, Alka Bali, Tanvi Gupta, Sudhanshu Shekhar

Idelalisib is a phosphatidylinositol 3-kinase delta inhibitor approved by the FDA and the EMA for the treatment of lympholytic lymphoma, B cell non-Hodgkin lymphoma, and lymphocytic lymphoma. The present report describes the validation of a simple, rapid, sensitive, and cost-effective zero-order and first-order derivative spectrophotometric method for the estimation of idelalisib in bulk and in its marketed formulation. Preliminary spectrophotometric analysis of the drug was carried out in methanol and a total of 12 parametric variations were considered. Three selected method variants employing peak-zero and peak-peak techniques were assessed for their stability indicating potential in stress degraded solutions of the drug. The developed method was validated with respect to linearity, accuracy, precision, and robustness. Excellent linearity was observed within the concentration range 1.0–60.0 μg/mL with a correlation coefficient of 0.9997. The limits of assay detection values were found for the range 0.42–3.11 μg/mL, and quantitation limits ranged from 1.29 to 9.42 μg/mL for the proposed method variants. The proposed method was used to quantify the drug in its marketed tablet formulation, and good recoveries ranging from 95.98 to 98.81% were obtained.

伊德拉利西是一种磷脂酰肌醇3-激酶δ抑制剂,经美国食品药品管理局(FDA)和欧洲药品管理局(EMA)批准用于治疗淋巴溶解性淋巴瘤、B细胞非霍奇金淋巴瘤和淋巴细胞淋巴瘤。本报告介绍了一种简单、快速、灵敏且经济有效的零阶和一阶导数分光光度法,用于估算散装和上市制剂中的伊德拉利西。在甲醇中对该药物进行了初步分光光度分析,共考虑了 12 种参数变化。所选的三种方法变体采用了峰-零和峰-峰技术,评估了它们在药物应力降解溶液中的稳定性和显示潜力。所开发的方法在线性、准确度、精密度和稳健性方面都得到了验证。在 1.0-60.0 μg/mL 的浓度范围内,线性关系良好,相关系数为 0.9997。该方法的检出限为 0.42-3.11 μg/mL,定量限为 1.29-9.42 μg/mL。采用所提出的方法对该药物的上市片剂进行了定量分析,获得了 95.98% 至 98.81% 的良好回收率。
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引用次数: 0
Redox State of Photosynthetic Ferredoxin Under Heat and Light Stress 光热胁迫下光合铁氧化还原酶的氧化还原状态
IF 0.8 4区 化学 Q4 SPECTROSCOPY Pub Date : 2024-05-13 DOI: 10.1007/s10812-024-01726-8
N. L. Pshybytko

The kinetics of oxidation/reduction of the primary donor of photosystem 1 (PS1) P700, plastocyanin (PC), and ferredoxin (Fd) in the first leaves of barley seedlings under exposure to high-intensity light (2000 μmol∙quanta∙m–2·s–1, 30 min) and elevated temperature (40°C, 3 h) were studied using differential absorption photometry. Exposure to high-intensity light increased the accumulation of the oxidized form of PS1 reaction center P700+, oxidized PC, and reduced Fd. Reduced Fd was not reoxidized under the same conditions on exposure to red and far-red light. The accumulation of P700+, PC+, and Fd increased in barley seedlings exposed to elevated temperatures. Also, reoxidation of leaf Fd accelerated under red light. Oxidized Fd did not accumulate under far-red light. It was concluded that photo-independent electron flow through Fd under light stress and alternative electron flows involving the plastoquinone pool under heat stress were activated.

利用差分吸收光度法研究了大麦幼苗在高强度光照(2000 μmol∙quanta∙m-2-s-1,30 分钟)和高温(40°C,3 小时)条件下第一片叶子中光合系统 1(PS1)主要供体 P700、质花青素(PC)和铁氧还蛋白(Fd)的氧化/还原动力学。暴露在高强度光下会增加 PS1 反应中心 P700+、氧化 PC 和还原 Fd 的氧化形式的积累。在红光和远红光照射的相同条件下,还原型 Fd 没有被再氧化。暴露在高温下的大麦幼苗中,P700+、PC+ 和 Fd - 的积累增加。此外,在红光照射下,叶片 Fd 的再氧化速度加快。氧化的 Fd 在远红光下没有积累。由此得出结论,在光胁迫下,通过 Fd 的不依赖于光的电子流被激活,而在热胁迫下,涉及质醌池的替代电子流被激活。
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引用次数: 0
Rapid Detection of Heavy Metal Ions Co3+, Cu2+, Ni2+, and Zn2+ in Wastewater By Pyrimidine–Thiourea Ligand 利用嘧啶-硫脲配体快速检测废水中的重金属离子 Co3+、Cu2+、Ni2+ 和 Zn2+
IF 0.8 4区 化学 Q4 SPECTROSCOPY Pub Date : 2024-05-13 DOI: 10.1007/s10812-024-01737-5
Zhou Wang, Feng Jin

Rapid detection of trace heavy metal ions in water is of great relevance to the environment and human health in the future. With pyrimidine as the parent structure, the water-soluble thiourea group is skillfully introduced to form a symmetric framework, thus firmly capturing the heavy metal ions in the water. The responsiveness of heavy metal ions in water was observed by UV-fluorescence spectroscopy. Especially with Co(NO3)2, Cu(NO3)2, Ni(NO3)2, and Zn(NO3)2, the response changes are most significant. The rapid response changes between them and trace heavy metal ions in water were intuitively observed under sunlight and fluorescence irradiation environment.

快速检测水中的痕量重金属离子与未来的环境和人类健康息息相关。以嘧啶为母体结构,巧妙地引入水溶性硫脲基团,形成对称框架,从而牢牢捕捉水中的重金属离子。紫外荧光光谱观察了水中重金属离子的响应性。尤其是对 Co(NO3)2、Cu(NO3)2、Ni(NO3)2 和 Zn(NO3)2 的反应变化最为显著。在阳光和荧光照射环境下,可以直观地观察到它们与水中痕量重金属离子之间的快速响应变化。
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引用次数: 0
Electrical Characteristics of p–i–n Mesa-Photodiodes Based on InGaAs/InP Heterostructures 基于 InGaAs/InP 异质结构的 pi-n Mesa-Photodiode 的电气特性
IF 0.8 4区 化学 Q4 SPECTROSCOPY Pub Date : 2024-05-11 DOI: 10.1007/s10812-024-01730-y
I. Gogorishvili, A. Tutunjyan, T. Sakharova, M. Melikyan, N. Khuchua, D. Kuparashvili

The current–voltage and capacitance–voltage characteristics of InGaAs/InP heterostructure p-i-n photodiodes fabricated by mesa technology have been studied. Photodiodes of circular configuration differ in active region diameter from 0.05 to 2.5 mm. All measurements are performed in the dark at room temperature using the probe method on a wafer with ready-made devices. Data are obtained on dark currents (leakage currents), Idark, which are interpreted in terms of the surface and bulk currents in p–i–n photodiodes of various sizes. In the absorbing layer of the InGaAs/InP photodiode heterostructures, the concentration profiles ND(x) are assessed for the first time by the nondestructive CV method and are compared with the electrochemical profiling data. It is shown that for the most part of the heterostructure i-layer the two methods are complementary.

研究了采用 mesa 技术制造的 InGaAs/InP 异质结构 pi-i-n 光电二极管的电流-电压和电容-电压特性。圆形结构的光电二极管有源区直径从 0.05 毫米到 2.5 毫米不等。所有测量都是在室温下的黑暗环境中,使用探针法在装有现成器件的晶片上进行的。我们获得了暗电流(漏电流)Idark 的数据,并根据不同尺寸 pi-n 光电二极管的表面电流和体积电流对这些数据进行了解释。在 InGaAs/InP 光电二极管异质结构的吸收层中,首次采用无损 CV 方法评估了浓度曲线 ND(x),并将其与电化学曲线数据进行了比较。结果表明,在异质结构 i 层的大部分区域,这两种方法是互补的。
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引用次数: 0
Luminescence Study and Energy Transfer from Ce3+ to Yb3+ in Sr5(BO3)3Cl Phosphor Sr5(BO3)3Cl 磷酸盐中的发光研究和从 Ce3+ 到 Yb3+ 的能量转移
IF 0.8 4区 化学 Q4 SPECTROSCOPY Pub Date : 2024-05-11 DOI: 10.1007/s10812-024-01732-w
R. A. Talewar

A new phosphor Sr5(BO3)3Cl:Ce3+,Yb3+, which enables near-infrared (NIR) quantum cutting, was prepared using traditional solid-state reaction methods. Its properties were examined using X-ray diffraction, photoluminescence emission, excitation spectra, and measurements of fluorescence decay. Upon excitation of Ce3+ with an ultraviolent (UV) photon at 350 nm, broadband emission at 415 nm and an intense NIR emission at 982 nm were observed. Emission at 415 nm corresponds to 5d→4f transition of Ce3+ ions, whereas the NIR emission at 982 nm is ascribed to the characteristic 2F5/22F7/2 transition of Yb3+ ions. Thorough investigation delved into how the concentration of Ce3+ affects visible and NIR emissions, decay lifetime, and energy transfer efficiency (ηETE). Detailed analysis of photoluminescence excitation, emission spectra, and fluorescence decay measurements revealed a proficient energy transfer from Ce3+ to Yb3+ ions. This transfer was demonstrated as a cooperative energy transfer (CET) process, showcasing a CET efficiency of 71.2% and a total theoretical quantum efficiency of 171.2%.

采用传统的固态反应方法制备了一种可实现近红外量子切割的新型荧光粉 Sr5(BO3)3Cl:Ce3+,Yb3+。研究人员利用 X 射线衍射、光致发光发射、激发光谱和荧光衰减测量方法考察了它的特性。用 350 纳米的紫外线(UV)光子激发 Ce3+ 时,可观察到 415 纳米的宽带发射和 982 纳米的强烈近红外发射。415 纳米波段的发射对应于 Ce3+ 离子的 5d→4f 转变,而 982 纳米波段的近红外发射则归因于 Yb3+ 离子特有的 2F5/2 → 2F7/2 转变。深入研究了 Ce3+ 的浓度如何影响可见光和近红外发射、衰变寿命和能量传递效率(ηETE)。对光致发光激发、发射光谱和荧光衰减测量结果的详细分析表明,Ce3+ 离子与 Yb3+ 离子之间存在着熟练的能量转移。这种能量转移被证明是一种协同能量转移(CET)过程,CET 效率为 71.2%,总理论量子效率为 171.2%。
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引用次数: 0
Effect of B2O3 on Optical Properties of Dy3+ Ion-Doped Zinc–Aluminum–Sodium–Phosphate Glasses B2O3 对掺杂 Dy3+ 离子的锌铝磷酸钠玻璃光学特性的影响
IF 0.8 4区 化学 Q4 SPECTROSCOPY Pub Date : 2024-05-11 DOI: 10.1007/s10812-024-01731-x
K. Brahmachary, G. Giribabu, Rajesh Dagupati, M. Dhamodhara Naidu

Different concentrations of B2O3 in zinc–aluminum–sodium–phosphate (ZANP) glasses were synthesized by the conventional melt-quenching method and analyzed using X-ray diffraction (XRD), optical absorption, excitation, visible luminescence, decay lifetime, and chromaticity methods. The amorphous nature of the glasses was confirmed by the absence of sharp diffraction peaks in the XRD profile. In the visible emission spectra blue, yellow, and red bands were observed and the intensity of the yellow band was superior. Furthermore, the samples show a luminescence quenching beyond 20 mol.% of B2O3 concentration. The decay lifetime of 4F9/2 of Dy3+ ions was found to be maximal in ZANP Dy0.5:20B2O3 glass.

采用传统的熔淬法合成了不同浓度的磷酸锌铝钠(ZANP)玻璃中的 B2O3,并使用 X 射线衍射(XRD)、光吸收、激发、可见光发光、衰减寿命和色度方法对其进行了分析。X 射线衍射曲线中没有尖锐的衍射峰,这证实了玻璃的无定形性质。在可见光发射光谱中观察到蓝色、黄色和红色条带,其中黄色条带的强度更高。此外,当 B2O3 浓度超过 20 摩尔/% 时,样品会出现发光淬灭现象。在 ZANP Dy0.5:20B2O3 玻璃中,Dy3+ 离子 4F9/2 的衰变寿命达到最大。
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引用次数: 0
NIR Inversion Model of Larch Wood Density at Different Moisture Contents Based on MVO-BPNN 基于 MVO-BPNN 的不同含水率下落叶松木材密度的近红外反演模型
IF 0.8 4区 化学 Q4 SPECTROSCOPY Pub Date : 2024-05-11 DOI: 10.1007/s10812-024-01743-7
Zhiyuan Wang, Zheyu Zhang, Roger A. Williams, Yaoxiang Li

Owing to variation of moisture content, the larch wood basic density near-infrared (NIR) prediction model shows reduced accuracy and robustness, or even model failure. To solve this technical problem, a multi-verse-algorithm-optimized BP neural network (MVO-BPNN) prediction model is proposed to improve the accuracy of the model. The preprocessing effects of the Savitzky–Golay smoothing, detrending, and 15-point moving average smoothing method were compared. The synergy interval partial least squares was used to extract the feature bands of the NIR spectra. Results showed that the prediction model based on MVO-BPNN was better than those based on BPNN and the genetic algorithm-optimized BPNN. It indicated that the NIR model based on the MVO-BPNN could effectively predict the basic density of wood with different moisture contents.

由于含水率的变化,落叶松木材基本密度近红外(NIR)预测模型的准确性和鲁棒性降低,甚至模型失效。为解决这一技术难题,提出了多逆算法优化 BP 神经网络(MVO-BPNN)预测模型,以提高模型的准确性。比较了萨维茨基-戈莱平滑法、去趋势法和 15 点移动平均平滑法的预处理效果。使用协同区间偏最小二乘法提取近红外光谱的特征波段。结果表明,基于 MVO-BPNN 的预测模型优于基于 BPNN 和遗传算法优化的 BPNN 预测模型。这表明基于 MVO-BPNN 的近红外模型可以有效地预测不同含水率木材的基本密度。
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引用次数: 0
Spectrophotometric Method Development and Validation of Empagliflozin in Active Pharmaceutical Ingredient and Tablet Dosage Form 活性药物成分和片剂中 Empagliflozin 的分光光度法开发与验证
IF 0.8 4区 化学 Q4 SPECTROSCOPY Pub Date : 2024-05-11 DOI: 10.1007/s10812-024-01734-8
Sagar Sahu, Ravindra Kumar Pandey, Shiv Shankar Shukla, Bina Gidwani

Empagliflozin, an inhibitor of SGLT-2, a sodium glucose co-transporter is found mainly in the proximal tubules of the nephronic components of the kidney. The assay of empagliflozin in its tablet form has been created using a unique, secure, and sensitive UV-spectrophotometric approach. During the development and validation of the method for the assay of empagliflozin, methanol was employed as the solvent. The maximum absorbance wavelength of the solution was determined by scanning in a UV spectrophotometer. At the specified wavelength; absorbance was measured using a variety of calibration standards. The linearity and range of the calibration curve of concentration vs. absorbance were computed. The accuracy, precision, limit of detection, limit of quantitation, and ruggedness of the analytical approach were among the metrics that were determined. A correlation coefficient of 0.999 indicated linearity within the concentration range 2–10 μg/mL. The maximum absorbance of empagliflozin in methanol was determined to be 238.5 nm. Recovery was estimated as per International Conference on Harmonization guidelines and was found to be as per the acceptance limits: 93.25%. The developed UV method was found to be precise with relative standard deviation less than 2%. The assessment of empagliflozin in its tablet formulation using a UV-spectrophotometric technique was determined to be both safe and helpful. The uniqueness of this research is based on a cost-efficient, time-saving, safe, easy, and successful approach for validating empagliflozin.

Empagliflozin 是钠葡萄糖共转运体 SGLT-2 的抑制剂,主要存在于肾脏近端肾小管中。采用独特、安全、灵敏的紫外分光光度法对片剂形式的 Empagliflozin 进行了检测。在开发和验证安帕格列净检测方法的过程中,使用了甲醇作为溶剂。通过紫外分光光度计扫描确定溶液的最大吸光波长。在指定波长下,使用各种校准标准测量吸光度。计算了浓度与吸光度校准曲线的线性和范围。确定了分析方法的准确度、精确度、检测限、定量限和耐用性等指标。相关系数为 0.999,表明在 2-10 μg/mL 浓度范围内呈线性关系。甲醇中恩帕格列净的最大吸光度为 238.5 纳米。根据国际协调会议准则对回收率进行了估算,发现回收率为 93.25%。所开发的紫外方法精确度高,相对标准偏差小于 2%。使用紫外分光光度法评估片剂中的恩格列净既安全又有帮助。这项研究的独特之处在于采用了一种经济、省时、安全、简便且成功的方法来验证安格列净。
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引用次数: 0
Rapid Identification and Classification of Metal Waste by Laser-Induced Breakdown Spectroscopy 利用激光诱导击穿光谱快速识别和分类金属废物
IF 0.8 4区 化学 Q4 SPECTROSCOPY Pub Date : 2024-05-11 DOI: 10.1007/s10812-024-01733-9
Zhuoyan Zhou, Wenhan Gao, Saifullah Jamali, Cong Yu, Yuzhu Liu

The rapid identification and classification of metal garbage has been experimentally investigated. By combining laser-induced breakdown spectroscopy (LIBS) and machine learning, metal garbage can be effectively identified through spectral analysis. In this work, a novel method for metal garbage classification was developed, and a LIBS system was self-developed. As an example of metal recycling, five types of metal were adopted. Several characteristic lines of Al, W, Fe, Cu, Sn, Pb, and C were identified. For a more effective classification, principal component analysis was conducted to reduce the dimension of the spectra. Samples after the dimension reduction were classified by using K-nearest neighbors, and five types were obtained, exhibiting a final classification accuracy of 97.18%. Moreover, a mathematical model of the linear formulas between spectrum and concentration was established to achieve quantitative analysis with Fe taken as an example, laying the foundation for more refined classification.

对金属垃圾的快速识别和分类进行了实验研究。将激光诱导击穿光谱(LIBS)与机器学习相结合,可以通过光谱分析有效识别金属垃圾。本研究开发了一种新型的金属垃圾分类方法,并自主研发了一套激光诱导击穿光谱系统。以金属回收为例,采用了五种金属。确定了 Al、W、Fe、Cu、Sn、Pb 和 C 的几条特征线。为了更有效地进行分类,进行了主成分分析以降低光谱的维度。利用 K 最近邻法对降维后的样本进行分类,得到五种类型,最终分类准确率为 97.18%。此外,以铁为例,建立了光谱与浓度之间线性公式的数学模型,实现了定量分析,为更精细的分类奠定了基础。
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引用次数: 0
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Journal of Applied Spectroscopy
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