盐酸度洛西汀的波谱学研究

报道并解析了盐酸度洛西汀的红外光谱、紫外光谱、质谱、氢-氢相关谱、碳谱(13C-NMR,DEPT)、碳氢相关谱、碳氢远程相关谱,对所有1HNMR和13CNMR谱的信号进行归属,同时讨论了红外特征吸收峰所对应的官能团的振动形式。     

Spectral data analysis and identification of Thymopentin

胸腺五肽的结构解析@于丽君$College of Clinical Medicine, Inner Mongolia University for Nationalities!Tongliao 028000, Inner Mongolia, China @张福中$Tongliao Entry-Exit Inspection and Quarantine Bureau!Tongliao 028000, Inner Mongolia ,China     

利塞膦酸钠的波谱学数据和结构确证

目的确证利塞膦酸钠的结构。方法采用红外（IR）、紫外（UV）、氢谱（1HNMR）、碳谱（13CNMR,DEPT）等进行结构解析。结果根据氢-氢相关谱（1H-1HCOSY）、碳氢相关谱（HMQC）、碳氢远程相关谱（HMBC）对所有的1HNMR和13CNMR谱信号进行了归属;讨论了红外特征吸收峰所对应的官能团的振动形式。结论确证了利塞膦酸钠的结构。     

胸腺五肽的波谱学解析与结构表征

目的为多肽类化合物的NMR解析提供理论基础和方法学依据。方法利用NMR、2D NMR及IR、UV、MS并借助1H-1H COSY1、3C-1H COSY及DEPT实验技术详细研究了胸腺五肽的结构特征。结果对胸腺五肽的氢谱和碳谱进行了完全归属。结论胸腺五肽的结构得到确认并为多肽类药物的结构解析提供了有益的分析依据。     

酒石酸唑吡坦红外光谱鉴别方法的探讨

目的:研究不同样品前处理方法对酒石酸唑吡坦原料药红外光谱分析的影响。方法:考察了氨水沉淀、25℃减压干燥、甲醇转晶和100℃干燥四种样品前处理方法对国内不同厂家生产的酒石酸唑吡坦原料药红外光谱分析和差示扫描量热(DSC)分析的影响。结果:红外光谱和DSC分析表明,氨水沉淀法通过将酒石酸唑吡坦转化为唑吡坦游离碱的方式消除多晶现象,25℃减压干燥和甲醇转晶均不能消除酒石酸唑吡坦的多晶现象,从而使不同厂家生产的原料药的红外光图谱在O-H、C=O和C=N的伸缩振动等区域产生差异,且DSC曲线分析均显示多个吸热峰。100℃干燥法处理后,不同厂家生产的原料药的红外光图谱和DSC曲线一致性好,且样品仍以酒石酸唑吡坦形式存在。结论:100℃干燥法能够消除酒石酸唑吡坦多晶现象对红外图谱分析的影响,是一种准确、高效的酒石酸唑吡坦的红外鉴别方法。     

Correlation between the free volume and the metoprolol tartrate release of Metolose patches

The correlation between the release characteristics of metoprolol tartrate and the free volumes of Metolose patches containing Metolose 90SH 100.000SR (hypromellose) and Metolose SM 4000 (methylcellulose) of various proportions was studied. Positron annihilation lifetime spectroscopy (PALS) measurements were performed in parallel with the metoprolol tartrate release study to track the free volume changes of patches. Second-order polynomial relationship was found, with good correlation, between the metoprolol tartrate released at the 6th hour, the o-positronium lifetime, indicating the free volume of the polymer, and the Metolose SM 4000 relative proportions. The main reason for this correlation is the change in the free volume size of the polymer patches embedding metoprolol tartrate as a function of the relative proportion of Metolose 90SH 100.000SR containing hydroxypropoxy substitution. Since there were no significant changes between the free volumes of Metolose polymers at any ratio of the constituents in the case of lack of metoprolol tartrate, the free volume changes refer to a possible intermolecular interaction between the polymer and the active agent.     

Raman spectroscopy for the in-line polymer-drug quantification and solid state characterization during a pharmaceutical hot-melt extrusion process

The aim of this study was to evaluate the suitability of Raman spectroscopy as a Process Analytical Technology (PAT) tool for the in-line determination of the active pharmaceutical ingredient (API) concentration and the polymer-drug solid state during a pharmaceutical hot-melt extrusion process.For in-line API quantification, different metoprolol tartrate (MPT) - Eudragit® RL PO mixtures, containing 10%, 20%, 30% and 40% MPT, respectively, were extruded and monitored in-line in the die using Raman spectroscopy. A PLS model, regressing the MPT concentrations versus the in-line collected Raman spectra, was developed and validated, allowing real-time API concentration determination. The correlation between the predicted and real MPT concentrations of the validation samples is acceptable (R² = 0.997). The predictive performance of the calibration model is rated by the root mean square error of prediction (RMSEP), which is 0.59%.Two different polymer-drug mixtures were prepared to evaluate the suitability of Raman spectroscopy for in-line polymer-drug solid state characterization. Mixture 1 contained 90% Eudragit® RS PO and 10% MPT and was extruded at 140 °C, hence producing a solid solution. Mixture 2 contained 60% Eudragit® RS PO and 40% MPT and was extruded at 105 °C, producing a solid dispersion. The Raman spectra collected during these extrusion processes provided two main observations. First, the MPT Raman peaks in the solid solution broadened compared to the corresponding solid dispersion peaks, indicating the presence of amorphous MPT. Second, peak shifts appeared in the spectra of the solid dispersion and solid solution compared to the physical mixtures, suggesting interactions between Eudragit® RS PO and MPT, most likely hydrogen bonds. These shifts were larger in the spectra of the solid solution. DSC analysis confirmed these Raman solid state observations and the interactions seen in the spectra. Raman spectroscopy is a potential PAT-tool for in-line determination of the API concentration and the polymer-drug solid state during pharmaceutical hot-melt extrusion.     

地黄配方颗粒高效液相色谱指纹图谱及红外图谱研究

目的建立地黄配方颗粒的高效液相色谱(HPLC)指纹图谱和红外光谱。方法分别采用HPLC和傅立叶变换红外光谱建立相应的HPLC指纹图谱和红外光谱。结果建立的HPLC指纹图谱和红外光谱专属性强。指纹图谱中,梓醇/毛蕊花糖苷(f)可区分地黄配方颗粒和熟地黄配方颗粒,且两者的红外二阶导数光谱差异较大,可选取不同的特征峰,以快速鉴别地黄配方颗粒和熟地黄配方颗粒。结论该方法能有效控制地黄配方颗粒的质量。     

美洛西林钠化学结构的确证

目的 建立美洛西林钠化学结构的确证方法。方法 通过热分析 ( TA )、元素分析( EA )、紫外吸收光谱( UV )、红外吸收光谱( IR )、核磁共振( NMR )以及质谱( MS )等分析手段对美洛西林钠样品进行结构分析。结果 证实了美洛西林钠的结构为(2S,5R,6R)-3,3-二甲基-6-[(2R)-[3-(甲磺酰基)-2-氧代-1-咪唑烷甲酰氨基]-2-苯乙酰氨基]-7-氧代-4-硫杂-1-氮杂双环[3.2.0]庚烷-2-甲酸钠盐。结论 该方法准确可行,可为美洛西林钠的生产和鉴定提供较全面的参考依据。     

光谱法鉴定黑海参中的多糖成分

目的:建立以光谱法鉴定黑海参中多糖成分的方法。方法:采用电泳法测定黑海参中多糖纯度,并用红外分光光度法、紫外分光光度法、核磁共振波谱法对其红外吸收光谱、紫外吸收光谱、核磁共振碳谱、核磁共振氢谱进行结构鉴定。结果:电泳后凝胶带呈蓝色,光谱检测结果可相互解释。结论:黑海参中存在均一组分的多糖成分,且为一种含硫酸酯基的酸性多糖,但不含糖肽;α-构型,存在α-吡喃葡萄糖,分子中的羟基形成分子内氢键。     

蒜氨酸精制品的纯化与结构确证

目的:制备蒜氨酸精制品并确证其结构.方法:采用反相制备液相和减压干燥技术制备高纯度的蒜氨酸精制品,用紫外光谱(UV)、红外(IR)、质谱(MS)、一维及二维核磁共振谱(1HNMR,13CNMR,1H-1HCOSY,DEPT,HSQC,HSBC)等波谱技术确证其化学结构,用旋光技术确定其立体构型.结果:蒜氨酸精制品的纯度为99.5%,所有的NMR谱信号均能得到合理的归属,质谱的裂解途径和离子特征也与蒜氨酸的分子结构相符,红外、紫外特征吸收峰均有合理的解释,比旋度测定结果与文献报道的S型蒜氨酸一致.结论:该制备方法可以得到高纯度的蒜氨酸精制品,其结构为S-烯丙基-L-半胱氨酸亚砜.     

Pharmacokinetic evaluation of guar gum-based three-layer matrix tablets for oral controlled delivery of highly soluble metoprolol tartrate as a model drug.

The objective of the present study is to carry out pharmacokinetic evaluation of oral controlled release formulation (guar gum-based three-layer matrix tablets) containing highly soluble metoprolol tartrate as a model drug. Six healthy volunteers participated in the study, and a two-way crossover design was followed. The plasma concentration of metoprolol tartrate was estimated by reverse-phase HPLC. The pharmacokinetic parameters were calculated from the plasma concentration of metoprolol tartrate versus time data. The delayed T(max) lower C(max) decreased K(a) unaltered bioavailability and prolonged t(1/2) indicated a slow and prolonged release of metoprolol tartrate from guar gum three-layer matrix tablets in comparison with the immediate release tablet dosage form. The results of the study indicated that guar gum three-layer matrix tablets were able to provide oral controlled delivery of highly water-soluble drug such as metoprolol tartrate in humans.     

Discrimination of Fritillary according to geographical origin with Fourier transform infrared spectroscopy and two-dimensional correlation IR spectroscopy

Fritillaria is a traditional Chinese herbal medicine for eliminating phlegm and relieving a cough with a long history in China and some other Asian countries. The objective of this study is to develop a nondestructive and accurate method to discriminate Fritillaria of different geographical origins, which is a troublesome work by existing analytical methods. We conducted a systematic study on five kinds of Fritillaria by Fourier transform infrared spectroscopy, second derivative infrared spectroscopy, and two-dimensional (2D) correlation infrared spectroscopy under thermal perturbation. Because Fritillaria consist of a large amount of starch, the conventional IR spectra of different Fritillaria only have very limited spectral feature differences. Based on these differences, we can separate different Fritillaria to a limited extent, but this method was deemed not very practical. The second derivative IR spectra of Fritillaria could enhance spectrum resolution, amplify the differences between the IR spectra of different Fritillaria, and provide some dissimilarity in their starch content, when compared with the spectrum of pure starch. Finally, we applied thermal perturbation to Fritillaria and analyzed the resulting spectra by the 2D correlation method to distinguish different Fritillaria easily and clearly. The distinction of very similar Fritillaria was possible because the spectral resolution was greatly enhanced by the 2D correlation spectroscopy. In addition, with the dynamic information of molecular structure provided by 2D correlation IR spectra, we studied the differences in the stability of active components of Fritillaria. The differences embodied mainly on the intensity ratio of the auto-peak at 985 cm(-1) and other auto-peaks. The 2D correlation IR spectroscopy (2D IR) of Fritillaria can be a new and powerful method to discriminate Fritillaria.     

近红外光谱快速鉴别金水宝胶囊的真伪

目的 利用近红外光谱快速鉴别金水宝胶囊的真伪.方法 在12000～4000 cm-1波段范围内对金水宝胶囊进行全谱扫描,并对图谱进行一阶倒数和矢量归一化处理.结果 正品金水宝胶囊与伪品金水宝胶囊的近红外光谱在7317～6927.5 cm-1、6738.5～6476.2 cm-1、5859～5523.4 cm-1范围内存在区别.结论 本方法简单、快速、准确,可应用于金水宝胶囊的日常监督打假.     

A three-layer guar gum matrix tablet for oral controlled delivery of highly soluble metoprolol tartrate

The objective of the study is to design oral controlled drug delivery systems for highly water-soluble drugs using guar gum as a carrier in the form of a three-layer matrix tablet. Metoprolol tartrate was chosen as a model drug because of its high water solubility. Matrix tablets containing either 30 (M1), 40 (M2) or 50% (M3) of guar gum were prepared by wet granulation technique using starch paste as a binder. Three-layer matrix tablets of metoprolol tartrate were prepared by compressing on both sides of guar gum matrix tablet granules of metoprolol tartrate M1, M2 or M3 with either 50 (TL1M1, TL1M2 or TL1M3) or 75 mg (TL2M1, TL2M2 or TL2M3) of guar gum granules as release retardant layers. Both the matrix and three-layer matrix tablets were evaluated for hardness, thickness, drug content uniformity, and subjected to in vitro drug release studies. The amount of metoprolol tartrate released from the matrix and three-layer matrix tablets at different time intervals was estimated by using a HPLC method. Matrix tablets of metoprolol tartrate were unable to provide the required drug release rate. However, the three-layer guar gum matrix tablets (TL2M3) provided the required release rate on par with the theoretical release rate for metoprolol tartrate formulations meant for twice daily administration. The three-layer guar gum matrix tablet (TL2M3) showed no change either in physical appearance, drug content or in dissolution pattern after storage at 40 degrees C/75% RH for 6 months. The FT-IR study did not show any possibility of metoprolol tartrate/guar gum interaction with the formulation excipients used in the study. The results indicated that guar gum, in the form of three-layer matrix tablets, is a potential carrier in the design of oral controlled drug delivery systems for highly water-soluble drugs such as metoprolol tartrate.     

Synthesis of copper nanoparticles as oxidising catalysts for multi-component reactions for synthesis of 1,3,4- thiadiazole derivatives at ambient temperature

Multi-component reactions (MCRs) are some of the most significant processes of highly functionalised organic compound synthesis in modern synthetic chemistry. This is a strong artifice for the rapid preparation of diverse heterocyclic scaffolds. This study involves two steps: first, fabricating copper nanoparticles as active catalysts using Trifolium resupinatum leaf extract as a reducing and capping agent and, second, utilising the active catalyst to synthesise 1,3,4-thiadiazole in a one-pot, three-component reaction via reacting with thiocarbohydrazide, acetophenone, and chalcone to produce 1,3,4-thiadiazole derivative compounds at an ambient temperature. Copper nanoparticles and T. resupinatum leaf extract have been characterised by ultraviolet–visible spectroscopy (UV-VIS), Fourier transform infrared (FTIR), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) spectrum, and pH analysis. The synthesised thiadiazole compounds have been identified by physical and spectral methods. The melting point, FTIR, UV-VIS, and ¹H, ¹³C NMR spectra were employed to verify the heterocyclic five-membered fused ring structure.     

巴戟天配方颗粒鉴别初步研究

目的为解决巴戟天配方颗粒在不具饮片外形后品种的真伪鉴别和质量优劣评价等重大技术问题。方法采用薄层色谱法、紫外光谱线组法和红外光谱法分别对不同批次的巴戟天配方颗粒进行研究。结果薄层色谱斑点清晰能与对照药材色谱对应;紫外光谱线组上的吸收峰数目及峰位值相同,重现性良好;红外光谱法操作简便,快捷,重现性良好。结论研究的方法可有效地控制巴戟天配方颗粒的质量。     

猪血中唾液酸的分离纯化工艺

猪血浆于80℃经酸水解后,用阳离子及阴离子交换树脂分离纯化、减压浓缩和冷冻干燥所得唾液酸成品,经薄层层析、紫外、红外光谱及质谱等确证,含量达88.8％。     

Has COMET solved the controversy as to whether carvedilol is better than metoprolol in heart failure?

Carvedilol and metoprolol are beta(1)-adrenoceptor antagonists that decrease mortality in heart failure. It is not clear whether the ancillary properties, which carvedilol has but metoprolol does not have, contribute to the beneficial effect. The Carvedilol Or Metoprolol European Trial (COMET) compared metoprolol tartrate (mean daily dose 85 mg) and carvedilol (41.8 mg) in patients with heart failure. All-cause mortality was less in the carvedilol than the metoprolol group, indicating that at these doses, carvedilol has a mortality benefit over metoprolol. However, the beta(1)-adrenoceptor blocking activity of metoprolol tartrate (assessed by a decrease in heart rate) was slightly less than with carvedilol in COMET and less than that observed in previous mortality studies with metoprolol, suggesting that the use of metoprolol tartrate was not optimal in COMET.     

Has COMET solved the controversy as to whether carvedilol is better than metoprolol in heart failure?

Carvedilol and metoprolol are β₁-adrenoceptor antagonists that decrease mortality in heart failure. It is not clear whether the ancillary properties, which carvedilol has but metoprolol does not have, contribute to the beneficial effect. The Carvedilol Or Metoprolol European Trial (COMET) compared metoprolol tartrate (mean daily dose 85 mg) and carvedilol (41.8 mg) in patients with heart failure. All-cause mortality was less in the carvedilol than the metoprolol group, indicating that at these doses, carvedilol has a mortality benefit over metoprolol. However, the β₁-adrenoceptor blocking activity of metoprolol tartrate (assessed by a decrease in heart rate) was slightly less than with carvedilol in COMET and less than that observed in previous mortality studies with metoprolol, suggesting that the use of metoprolol tartrate was not optimal in COMET.