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Estimation of Tadalafil Using Derivative Spectrophotometry in Bulk Material and in Pharmaceutical Formulation 导数分光光度法测定原料药和制剂中他达拉非的含量
Pub Date : 2014-05-21 DOI: 10.1155/2014/392421
Z. Khan, A. Patil, A. Shirkhedkar
Four simple, rapid, accurate, precise, reliable, and economical UV-spectrophotometric methods have been proposed for the determination of tadalafil in bulk and in pharmaceutical formulation. “Method A” is first order derivative UV spectrophotometry using amplitude, “method B” is first order derivative UV spectrophotometry using area under curve technique, “method C” is second order derivative UV spectrophotometry using amplitude, and “method D” is second order derivative UV spectrophotometry using area under curve technique. The developed methods have shown best results in terms of linearity, accuracy, precision, and LOD and LOQ for bulk drug and marketed formulation as well. In N,N-dimethylformamide, tadalafil showed maximum absorbance at 284 nm. For “method A” amplitude was recorded at 297 nm while for “method B” area under curve was integrated in the wavelength range of 290.60–304.40 nm. For “method C” amplitude was measured at 284 nm while for “method D” area under curve was selected in the wavelength range of 280.80–286.20 nm. For methods A and B, tadalafil obeyed Lambert-Beer’s law in the range of 05–50 μg/mL while for “methods C and D”, tadalafil obeyed Lambert-Beer’s law in the range of 20–70 μg/mL, and-for “methods A, B, C, and D” the correlation coefficients were found to be  than 0.999.
建立了四种简便、快速、准确、精密度、可靠、经济的紫外分光光度法测定原料药和制剂中他达拉非的方法。“方法A”是采用幅度法的一阶导数紫外分光光度法,“方法B”是采用曲线下面积法的一阶导数紫外分光光度法,“方法C”是采用幅度法的二阶导数紫外分光光度法,“方法D”是采用曲线下面积法的二阶导数紫外分光光度法。所开发的方法在原料药和上市制剂的线性度、准确度、精密度以及LOD和LOQ方面均显示出最佳结果。在N,N-二甲基甲酰胺中,他达拉非在284 nm处的吸光度最大。方法A在297 nm处记录振幅,方法B在290.60 ~ 304.40 nm范围内积分曲线下面积。方法C在284 nm处测量振幅,方法D在280.80 ~ 286.20 nm范围内选择曲线下面积。方法A、B在05 ~ 50 μg/mL范围内符合兰伯特-比尔定律,方法C、D在20 ~ 70 μg/mL范围内符合兰伯特-比尔定律,方法A、B、C、D的相关系数均大于0.999。
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引用次数: 11
FTIR Spectroscopy Combined with Partial Least Square for Analysis of Red Fruit Oil in Ternary Mixture System FTIR光谱结合偏最小二乘法分析三元混合体系中的红果油
Pub Date : 2014-05-21 DOI: 10.1155/2014/785914
A. Rohman, D. L. Setyaningrum, S. Riyanto
FTIR spectroscopy is a promising method for quantification of edible oils. Three edible oils, namely, red fruit oil (RFO), corn oil (CO), and soybean oil (SO), in ternary mixture system were quantitatively analyzed using FTIR spectroscopy in combination with partial least square (PLS). FTIR spectra of edible oils in ternary mixture were subjected to several treatments including normal spectra and their derivative. Using PLS calibration, the first derivative FTIR spectra can be exploited for determination of RFO; meanwhile, the second derivative spectra were preferred for determination of CO and SO. The values obtained for the relationship between actual and FTIR predicted values of RFO, CO, and SO were 0.9863, 0.9276, and 0.9693, respectively. The root mean square error of calibration (RMSEC) values obtained were 1.59, 1.72, and 1.60% (v/v) for RFO, CO, and SO, respectively. The result showed that FTIR spectroscopy offers accurate and reliable technique for quantitative analysis of RFO, CO, and SO simultaneously in ternary mixture systems. Besides, the developed method can be extended for analysis of CO and SO as adulterants in RFO.
FTIR光谱法是一种很有前途的食用油定量方法。采用偏最小二乘法(PLS)对三元混合体系中的红果油(RFO)、玉米油(CO)和大豆油(SO) 3种食用油进行了定量分析。对三元混合物中食用油的红外光谱进行了常规光谱及其衍生物的处理。利用PLS校准,一阶导数FTIR光谱可用于RFO的测定;同时,二阶导数光谱更适合于CO和SO的测定。RFO、CO、SO的实际预测值与FTIR预测值的关系分别为0.9863、0.9276、0.9693。RFO、CO和SO的校准均方根误差(RMSEC)值分别为1.59、1.72和1.60% (v/v)。结果表明,FTIR光谱技术为同时定量分析三元混合体系中的RFO、CO和SO提供了准确可靠的技术。此外,所建立的方法也可推广应用于RFO中CO和SO的掺假分析。
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引用次数: 24
Simple Atomic Absorption Spectroscopic and Spectrophotometric Methods for Determination of Pioglitazone Hydrochloride and Carvedilol in Pharmaceutical Dosage Forms 简单原子吸收光谱法和分光光度法测定制剂中盐酸吡格列酮和卡维地洛的含量
Pub Date : 2014-05-18 DOI: 10.1155/2014/768917
A. A. Abdelmonem, G. Ragab, H. Hashem, E. Bahgat
This study represents simple atomic absorption spectroscopic and spectrophotometric methods for determination of pioglitazone hydrochloride (PGZ-HCl) and carvedilol (CRV) based on formation of ion-pair associates between drugs and inorganic complex, bismuth(III) tetraiodide (Method A) and between drugs and organic acidic dyes, fast green and orange G (Method B). Method A is based on formation of ion-pair associate between drugs and bismuth(III) tetraiodide in acidic medium to form orange-red ion-pair associates, which can be quantitatively determined by two different procedures. The formed ion-pair associate is extracted by methylene chloride, dissolved in acetone, dried, and then decomposed by hydrochloric acid, and bismuth content is determined by direct atomic absorption spectrometric technique (Procedure 1) or extracted by methylene chloride, dissolved in acetone, and quantified spectrophotometrically at 490 nm (Procedure 2). Method B is based on formation of ion-pair associate between drugs and either fast green dye or orange G dye in acidic medium to form ion-pair associates. The formed ion-pair associate is extracted by methylene chloride and quantified spectrophotometrically at 630 nm (for fast green dye method) or 498 nm (for orange G dye method). Optimal experimental conditions have been studied. Both methods are applied for determination of the drugs in tablets without interference.
本研究基于药物与无机配合物四碘化铋(方法A)之间以及药物与有机酸性染料之间形成离子对,建立了简单的原子吸收光谱和分光光度法测定盐酸吡格列酮(PGZ-HCl)和卡维地洛(CRV)的方法。快速绿色和橙色G(方法B)。方法A是基于药物与四碘化铋(III)在酸性介质中形成离子对缔合物,形成橙红色离子对缔合物,可通过两种不同的方法定量测定。形成的离子对缔合物用二氯甲烷萃取,溶解在丙酮中,干燥,然后用盐酸分解,用直接原子吸收光谱法(程序1)测定铋含量或用二氯甲烷萃取,溶解在丙酮中,方法B是基于在酸性介质中药物与快速绿色染料或橙色G染料之间形成离子对缔合物以形成离子对缔合物。形成的离子对通过二氯甲烷萃取并在630 nm(快速绿色染料法)或498 nm(橙色G染料法)处进行定量。研究了最佳实验条件。两种方法均可用于片剂中药物的测定,无干扰。
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引用次数: 5
Two-Pulse Phase Modulation Based Decoupling Schemes for Removing Heteronuclear Spin Interactions in the NMR Spectroscopy ofIsotropic Systems: An Analysis Using Experiments and Numerical Simulations 基于双脉冲相位调制的解耦方案消除各向同性系统核磁共振波谱中的异核自旋相互作用:实验和数值模拟分析
Pub Date : 2014-05-15 DOI: 10.1155/2014/641473
Cyril Augustine
Heteronuclear spin interactions in solids and anisotropic liquids can be removed by phase modulated decoupling sequences with frequency sweep, such as -TPPM and its variants. The performance of these sequences in isotropic spin systems with regard to the experimental parameters, phase angle, and decoupler offset is presented here. A comparison is made with other commonly used heteronuclear decoupling schemes in liquids, namely, WALTZ-16, GARP, and MLEV. Also, the trajectories of nuclear magnetization vector of abundant nuclei in a simple spin system during TPPM and -TPPM decoupling sequences are traced out using computer simulations.
固体和各向异性液体中的异核自旋相互作用可以通过带频率扫描的相位调制解耦序列去除,例如-TPPM及其变体。本文给出了这些序列在各向同性自旋系统中与实验参数、相位角和解耦偏移有关的性能。并与其他常用的液体异核解耦方案,即华尔兹-16、GARP和MLEV进行了比较。此外,利用计算机模拟,我们还得到了简单自旋系统中富核在TPPM和-TPPM解耦过程中的核磁化矢量轨迹。
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引用次数: 0
New Simple Spectrophotometric Method for the Simultaneous Estimation of Paracetamol and Flupirtine Maleate in Pure and Pharmaceutical Dosage Form 新的简单分光光度法同时测定纯剂型和药用剂型对乙酰氨基酚和马来酸氟吡汀的含量
Pub Date : 2014-05-12 DOI: 10.1155/2014/968420
P. Giriraj, T. Sivakkumar
A new, simple, precise, accurate, reproducible, and efficient Vierordt’s method or simultaneous equation method was developed and validated for simultaneous estimation of paracetamol and flupirtine maleate in pure and pharmaceutical dosage form. The method was based on the measurement of absorbance at two wavelengths 245 nm and 344.5 nm, of paracetamol and flupiritine maleate in 0.1 N HCl correspondingly. Calibration curves of paracetamol and flupiritine maleate were found to be linear in the concentration ranges of 5–15 μg/mL and 1.53–4.61 μg/mL, respectively, with their correlation coefficient values (R2) 0.999. LOD and LOQ were 185.90 ng/mL and 563.38 ng/mL for paracetamol and 78.89 ng/mL and 239.06 ng/mL for flupiritine maleate. In the precision study, the % RSD value was found within limits (%). The percentage recovery at various concentration levels varied from 99.18 to 100.02% for paracetamol and 98.47 to 100.09% for flupiritine maleate confirming that the projected method is accurate. It could be concluded from the results obtained in the present investigation that this method for simultaneous estimation of paracetamol and flupirtine maleate in pure and tablet dosage form is simple, accurate, precise, and economical. The proposed method can be applied successfully for the simultaneous estimation of paracetamol and flupiritine maleate in pure and pharmaceutical dosage form.
建立了一种简便、精确、准确、重现性好、高效的Vierordt法或联立方程法,用于同时测定纯剂型和药用剂型对乙酰氨基酚和马来酸氟吡汀的含量。该方法是通过测定对乙酰氨基酚和马来酸氟吡替汀在0.1盐酸溶液中245nm和344.5 nm两个波长的吸光度来实现的。对乙酰氨基酚和马来酸氟吡替汀在5 ~ 15 μg/mL和1.53 ~ 4.61 μg/mL范围内与标度曲线分别呈良好的线性关系,相关系数(R2)为0.999。对乙酰氨基酚的LOD和LOQ分别为185.90 ng/mL和563.38 ng/mL,马来酸氟吡替汀的LOD和LOQ分别为78.89 ng/mL和239.06 ng/mL。在精密度研究中,发现% RSD值在限定范围内(%)。在不同浓度下,对乙酰氨基酚的回收率为99.18% ~ 100.02%,马来酸氟吡汀的回收率为98.47 ~ 100.09%,验证了预测方法的准确性。本研究结果表明,该方法简便、准确、精密度高、经济,可同时测定对乙酰氨基酚和马来酸氟吡汀纯剂型和片剂剂型的含量。该方法可成功地同时测定纯剂型和药用剂型对乙酰氨基酚和马来酸氟吡替汀的含量。
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引用次数: 17
Spectroscopic Characterization of Stability and Interaction of Pd-Ag Complexes 钯银配合物稳定性及相互作用的光谱表征
Pub Date : 2014-05-08 DOI: 10.1155/2014/314070
Sharad V. Lande, Nagesh Sharma, Ajay Kumar, R. Jasra
Colloidal metal nanoparticles are of great interest because of their use as catalysts, photocatalysts, adsorbents, and sensors as well as their application in optical, electronic, and magnetic devices. Supported bimetallic systems represent a large part of heterogeneous catalysts which have been used in various reactions important in the chemical, petrochemical, and oil industry. Pd-Ag bimetallic nanocatalysts have become vitally important in some of the petrochemical industry’s processes like hydrogenation of C2–C5 olefins. A heat-treatment method for the preparation of well-stable Pd-Ag complexes is demonstrated using water, concentrated HCl and concentrated nitric acid as media. The stability and interaction of Pd-Ag complexes were characterized by UV-vis absorption spectroscopy. Pd-Ag bimetallic nanoparticles of spherical cubic and octahedral shape in the range of average particle size of 20–60 nm have been prepared and characterized by transmission electron microscopy (TEM).
胶体金属纳米颗粒由于其作为催化剂、光催化剂、吸附剂和传感器以及在光学、电子和磁性器件中的应用而引起了人们的极大兴趣。负载双金属系统代表了非均相催化剂的很大一部分,在化学、石化和石油工业的各种重要反应中得到了应用。钯银双金属纳米催化剂在石化工业的一些过程中已变得至关重要,如C2-C5烯烃的加氢。以水、浓盐酸和浓硝酸为介质,研究了一种制备稳定性良好的钯银配合物的热处理方法。用紫外-可见光谱法对钯银配合物的稳定性和相互作用进行了表征。制备了平均粒径在20 ~ 60 nm之间的球立方和八面体形状的钯银双金属纳米颗粒,并用透射电镜对其进行了表征。
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引用次数: 1
The Application of Simple and Easy to Implement Decoupling Pulse Scheme Combinations to Effect Decoupling of Large Values with Reduced Artifacts 应用简单易实现的解耦脉冲方案组合在减少伪影的情况下实现大值解耦
Pub Date : 2014-04-29 DOI: 10.1155/2014/289638
K. Klika
Of the various problems in decoupling one nucleus type from another using standard decoupling pulse schemes for broadband decoupling, a particular challenge is to effect full, artifact-free decoupling when the size of the coupling constant is very large. Herein it is demonstrated that 1H decoupling of the 31P NMR spectrum of diethyl phosphonate HP(=O)(OCH2CH3)2 can be accomplished with reduced artifacts despite the large value of 693 Hz by using a combination of decoupling pulse schemes involving continuous-wave (CW) irradiation and either adiabatic-pulse decoupling (APD), MPF decoupling, or traditional composite-pulse decoupling (CPD) schemes such as WALTZ or GARP. The considered strategy is simple, efficient, and easy to implement on most instruments. The best result was attained for a combination of CW and CPD using GARP with a standard pulse width of 60 μs. Altogether, the advantages of the methodology include low power requirements, complete decoupling, tolerance of a range of large values, large bandwidth for normal-sized values, and the suppression of sidebands.
在宽带解耦中使用标准解耦脉冲方案将一种核类型从另一种核类型解耦的各种问题中,一个特别的挑战是当耦合常数的大小非常大时实现完全的、无伪影的解耦。本文证明,使用连续波(CW)照射和绝热脉冲解耦(APD)、MPF解耦或传统复合脉冲解耦(CPD)方案(如WALTZ或GARP)的组合,可以实现磷酸二乙酯HP(=O)(OCH2CH3)2的31P核磁共振谱的1H解耦,尽管693 Hz的值很大。所考虑的策略简单、有效,并且易于在大多数仪器上实现。在标准脉冲宽度为60 μs的GARP条件下,连续波和连续波的结合效果最好。总之,该方法的优点包括低功耗要求、完全解耦、大值范围的容限、标准尺寸值的大带宽以及侧带的抑制。
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引用次数: 13
Development and Validation of a Discriminating In Vitro Dissolution Method for Oral Formulations Containing Satranidazole 沙硝唑口服制剂体外溶出度鉴别方法的建立与验证
Pub Date : 2014-04-24 DOI: 10.1155/2014/624635
H. Pawar, P. Joshi
The development of a meaningful dissolution procedure for drug products with limited water solubility has been a challenge to the pharmaceutical industry. Satranidazole (BCS Class II drug) is a new nitroimidazole derivative with potent antiamoebic action. There is no official dissolution medium available in the literature. In the present study, parameters such as saturation solubility in different pH medium, dissolution behavior of formulations, influence of sink conditions, stability, and discriminatory effect of dissolution testing were studied for the selection of a proper dissolution medium. Results of solubility data revealed that solubility of Satranidazole decreases with an increase in pH. Satranidazole showed better sink condition in 0.1 N HCl as compared to other media. The drug and marketed formulations were stable in the dissolution media used. An agitation speed of 75 rpm showed a more discriminating drug release profile than 50 rpm. Using optimized dissolution parameters (paddle at 75 rpm, 900 mL 0.1 N HCl) greater than 80% of the label amount is released over 60 minutes. UV-spectroscopic method used was validated for the specificity, linearity, precision, robustness, and solution stability. The method was successfully applied to granular formulations and also to marketed tablets containing 300 mg Satranidazole.
开发具有有限水溶性的药品有意义的溶出程序一直是制药工业面临的挑战。Satranidazole (BCS II类药物)是一种新的硝基咪唑衍生物,具有有效的抗阿米巴作用。文献中没有官方的溶解介质。本文研究了不同pH介质的饱和溶解度、配方的溶解行为、沉淀条件的影响、稳定性和溶解试验的判别效应等参数,以选择合适的溶解介质。溶解度数据表明,随着ph的增加,Satranidazole的溶解度降低,在0.1 N HCl中,Satranidazole的沉降条件较其他介质好。该药物和市售制剂在所使用的溶出介质中是稳定的。75转/分的搅拌速度比50转/分的搅拌速度更能鉴别药物释放。使用优化的溶解参数(桨速75 rpm, 900 mL 0.1 N HCl),大于80%的标签量在60分钟内释放。验证了紫外光谱法的特异性、线性度、精密度、鲁棒性和溶液稳定性。该方法成功地应用于颗粒制剂和市场上销售的含有300 mg沙硝唑的片剂。
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引用次数: 8
Structural Characterization of Amadori Rearrangement Product of Glucosylated Nα-Acetyl-Lysine by Nuclear Magnetic Resonance Spectroscopy 糖基化n - α-乙酰赖氨酸Amadori重排产物的核磁共振谱结构表征
Pub Date : 2014-04-17 DOI: 10.1155/2014/789356
Chuanjiang Li, Hui Wang, M. Juárez, E. Ruan
Maillard reaction is a nonenzymatic reaction between reducing sugars and free amino acid moieties, which is known as one of the most important modifications in food science. It is essential to characterize the structure of Amadori rearrangement products (ARPs) formed in the early stage of Maillard reaction. In the present study, the Nα-acetyl-lysine-glucose model had been successfully set up to produce ARP, Nα-acetyl-lysine-glucose. After HPLC purification, ARP had been identified by ESI-MS with intense [M
美拉德反应是还原糖和游离氨基酸之间的一种非酶促反应,是食品科学中最重要的修饰之一。对美拉德反应早期形成的Amadori重排产物(ARPs)的结构进行表征是十分必要的。在本研究中,成功建立了n - α-乙酰赖氨酸-葡萄糖生成ARP模型,n - α-乙酰赖氨酸-葡萄糖。高效液相色谱纯化后,用ESI-MS对ARP进行鉴定
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引用次数: 11
The Low Energy Auger Electron Spectroscopy Lines as an Index of the Ba Overlayer Order on the Ni(110) Surface 低能俄歇能谱线作为Ni(110)表面Ba层序的指标
Pub Date : 2014-03-26 DOI: 10.1155/2014/289346
D. Vlachos, M. Kamaratos, S. Foulias
We investigate the interaction of Ba with the Ni(110) surface at elevated temperatures by means of Auger electron spectroscopy and low energy electron diffraction. The results show that annealing of the substrate causes desorption and ordering of the initially amorphous overlayer, resulting in c and structures. It is observed that the induced ordering crucially affects the lineshape of the double Auger transition line Ba(73 eV)N45O23P1, establishing this line as an index of ordering of the Ba overlayer. The underlying physics of this effect is discussed.
利用俄歇电子能谱和低能电子衍射研究了高温下Ba与Ni(110)表面的相互作用。结果表明:衬底的退火使初始非晶层脱附有序,形成c和结构;观察到诱导有序对双俄歇过渡线Ba(73 eV)N45O23P1的线形有重要影响,并将其作为Ba层有序的指标。讨论了这种效应的基本物理原理。
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引用次数: 0
期刊
International Journal of Spectroscopy
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