帕拉米韦及其中间体酯化物结构的X射线衍射分析

目的 验证所合成的化合物为目标产物——帕拉米韦中间体酯化物及帕拉米韦成品,并通过X射线衍射技术探讨化合物晶型.方法 选择适宜的条件,培养出适合单晶X射线衍射分析的单晶体,对所得单晶数据进行结构解析,得到化合物的三维空间结构信息,与文献进行比对;同时通过单晶结构数据模拟获得化合物的粉末X射线衍射理论图谱,用于晶型研究.结果 单晶X射线衍射结构分析结果表明,帕拉米韦中间体酯化物及成品的化学结构、构型与文献报道完全一致:粉末X射线衍射理论图谱可作为晶型对照图谱使用,并进一步表明中间体存在多晶型现象.结论 单晶X射线衍射分析法可准确测定含多手性中心的帕拉米韦中间体酯化物及成品的空间结构,充分证实了该药物合成过程与结果的正确性;粉末X射线衍射理论图谱可为化合物晶型研究提供有力支持.     

金莲花的X射线荧光分析及X射线衍射技术研究

目的：建立金莲花中药材内在质量的快速鉴别方法。方法：采用X射线荧光分析方法（XRF）和粉末X射线衍射技术（PXRD）对5个不同来源及产地金莲花样品的元素含量和整体特征进行了测定和分析。结果：5个样品中钾和钙元素含量均较高；而微量元素含量差异较大；道地品中富含钾元素的晶态物质含量最高，晶粒尺寸却最小，约40nm。结论：首次在金莲花中发现了富钾相。2种方法的联合应用不仅可以表达和鉴别药材的产地特征及识别其优劣；也能用于可制成粉末样品的中成药的鉴别、表征和质量控制，而且在质量标准的研究及制定方面具有广阔应用前景。     

生牡蛎X射线衍射分析及指纹图谱的建立

目的:建立生牡蛎的X射线衍射指纹图谱,考察X射线衍射分析在生牡蛎质量检测与鉴别中的应用价值。方法:应用X射线衍射法对11批生牡蛎样品进行定性分析,比较其共有峰的夹角余弦和相关系数的相似度。结果:各生牡蛎样品X射线衍射共有峰的相似度均达到95%以上。结论:生牡蛎的X射线衍射分析方法专属性强、准确可靠,能全面、客观地反映其内在质量特征。     

注射用青霉素钠的X射线衍射分析

目的建立注射用青霉素钠的新鉴定分析方法。方法应用X射线衍射分析方法,对不同来源的注射用青霉素钠共5批进行X射线衍射分析鉴别。结果注射用青霉素钠的X射线衍射图谱中均可检出青霉素钠的特征峰。结论 X射线衍射分析可用于注射用青霉素钠的鉴定。     

青天葵X射线衍射Fourier指纹图谱的建立及相似度分析

目的:建立青天葵X-射线衍射Fourier(傅立叶)指纹图谱,并对不同产地该药材进行相似度分析。方法:应用粉末X-射线衍射法,通过对8批青天葵药材进行分析,建立青天葵X-射线衍射Fourier指纹图谱,并进行相似度评价。结果:获得了青天葵X-射线衍射Fourier指纹图谱、特征标记峰值和相似度。结论:X-射线衍射Fourier指纹图谱专属性强,可用于中药青天葵的鉴定。     

矿物药玄精石的X射线衍射鉴定研究

目的:建立矿物药玄精石的新鉴定分析方法.方法:采用粉末X射线衍射Fourier谱鉴定法,对7批收集于全国不同地区的玄精石样品进行扫描、分析.结果:获得了玄精石的标准X射线衍射Fourier图谱及特征标记峰值.结论:X射线衍射Fourier谱鉴定法可用于矿物药玄精石的鉴定.     

X射线衍射分析法鉴定注射用头孢曲松钠

目的:建立注射用头孢曲松钠的鉴定分析方法。方法:采用X射线衍射分析方法。对7厂家的注射用头孢曲松钠进行测定并得到X射线衍射图谱,并与头孢曲松标准品及标准图谱进行对比分析。结果:各厂家注射用头孢曲松钠的X射线衍射图谱与标准品及标准图谱结果一致,均可检出头孢曲松钠特征峰。结论:X射线衍射分析方法简便、准确,可用于注射用头孢曲松钠的鉴定。     

应用粉末X射线衍射法测定地氯雷他定中晶型Ⅰ和晶型Ⅱ的比例

目的：用粉末X射线衍射法测定地氯雷他定原料中晶型Ⅰ和晶型Ⅱ所占重量百分比。方法：将晶型Ⅰ和晶型Ⅱ对照品按照5种不同比例混合后测定,以二者特征峰面积比对重量比绘制标准曲线,采用内标法和标准加入法相结合的方法计算两种晶型所占重量百分比。结果：线性方程为y=2.3205x-1.5641,r=0.9986,3批样品中晶型Ⅰ和晶型Ⅱ的百分比分别为94.8%,5.2%;94.5%,5.5%;92.8%,7.2%。结论：粉末X衍射法可以用于地氯雷他定中晶型Ⅰ和晶型Ⅱ的定量分析。     

中药材血竭的X衍射Fourier谱分析

采用粉末X衍射法,对3个血竭样品进行分析,获得了血竭的标准X衍射Fourier因语及特征标记峰,表明此法在中药材鉴定中有着广阔的应用前景。     

苍术X射线衍射Fourier特征图谱鉴定

目的:探索中药材苍术新的鉴定方法。方法:运用粉末X射线衍射Fourier特征图谱法对苍术药材进行扫描分析。结果:对8份不同产地苍术饮片及苍术对照药材进行分析,获得了苍术的X射线衍射Fourier特征图谱及特征标记峰。结论:苍术的X射线衍射Fourier谱重复性好、特征性强,具有指纹特征,可作为鉴别指标。经X射线衍射Fourier谱对比分析,南、北苍术的衍射图谱几何拓扑特征有明显差异。     

Thermal and X-ray powder diffraction structural characterization of two benfluorex hydrochloride polymorphs

Two polymorphic forms of benfluorex hydrochloride, phases I and II, were isolated as monophasic polycrystalline samples, and structurally characterized using ab initio X-ray powder diffraction methods and a global optimization strategy (simulated annealing). Form I crystallizes in monoclinic system, space group P2₁/n, with Z = 4, a = 21.0719(10) Å, b = 7.0563(4) Å, c = 14.8684(7) Å, β = 116.998(3)°, V = 1969.8(2) Å³, while Form II crystallizes in the orthorhombic space group Pbca, with Z = 8, a = 33.8031(2) Å, b = 15.1451(8) Å, c = 7.6138(6) Å, V = 3897.9(4) Å³. Crystals of Form I and Form II of benfluorex hydrochloride are based upon an ionic packing of protonated benfluorex molecules at the most basic site, the N1 atoms, and chloride anions. Form I shows the presence of μ-Cl ions, generating centrosymmetric dimers with a N₂Cl₂ moiety, while Form II contains antiparallel chains of C–H?O hydrogen-bonded molecules running along c axis. DSC and thermodiffractometric measurements showed that heating progressively Form II from ambient temperature to 160 °C causes a phase transition to the thermodynamically stable Form I, immediately followed by the sample melting, near 165 °C. Recrystallization directly to Form I is observed when the melt is cooled back to ambient temperature, with a significant hysteresis (this event being centered near 130 °C).     

Quantification of olanzapine polymorphs using powder X-ray diffraction technique

Accurate quantification of crystalline phases present in drug materials is becoming increasingly important, due to stringent regulatory concerns about polymorph characterization and control in drug substances and products. In the present study, a quantification method for polymorphic forms of olanzapine (OLZ) has been developed using powder X-ray diffraction (PXRD). Preferred orientation has been reported to be the major source of error in PXRD analysis, therefore, prior to development of a quantification method, pure polymorphic forms (I and II) of different size ranges were analyzed. Preferred orientation effect was found to decrease on using sieve fraction BSS # 120/240 for form I. In order to obtain good peak resolution in optimum time, the step time and step size were varied so as to optimize the scan rate. Among the five combinations selected, step size of 0.05 degrees with step time of 5s demonstrated identification of four characteristic peaks of form I in form II in 62 min. A calibration curve was constructed in the range of 0-100% (w/w) using the characteristic peak of form I at 18.48 degrees 2theta (I/I(0) 78.8%). The PXRD assay was reproducible and precise and displayed a LOD of 0.40% (w/w) and LOQ of 1.22% (w/w). Validation results showed excellent correlation between actual and predicted concentrations with R(2) 0.9999.     

中药紫石英X-衍射Fourier指纹图谱鉴别研究

目的:建立中药紫石英X-衍射Fourier指纹图谱。方法:对10批主产地的紫石英药材X-衍射Fourier图谱进行分析,建立中药紫石英X-衍射Fourier指纹图谱,并通过相似度计算,区分紫石英、紫石英混淆品、同种化学试剂CaF2。结果:中药紫石英X-衍射Fourier指纹图谱具有很好的专属性,与紫石英混淆品、同种化学试剂CaF2的X-衍射Fourier图谱区别显著。结论:中药紫石英X-衍射Fourier指纹图谱可全面地、客观地反映出紫石英的内在质量特征,可作为紫石英质量检测与鉴别的手段。     

不同茎叶比例的穿心莲药材中穿心莲内酯与脱水穿心莲内酯的X射线衍射定量分析方法的探讨

穿心莲中药材为爵床科植物穿心莲Andrographis paniculata(Burm.f.)Nees的干燥地上部分。秋初茎叶茂盛时采割,晒干。性味苦、寒,归心、肺、大肠、膀胱经,具有清热解毒、凉血、消肿的功能。穿心莲属常用中药材,穿心莲内酯与脱水穿心莲内酯作为     

市售生、煅炉甘石的成分分析及质量评价

目的:对市售矿物药生、煅炉甘石进行成分分析和质量评价。方法:采用X射线衍射(XRD)法对17批生炉甘石和13批煅炉甘石样品进行成分分析,并按2005年版《中国药典》规定方法测定ZnO含量。结果:市售生、煅炉甘石XRD谱显示其多为CaCO3及其它杂质而无应有的ZnCO3或ZnO。结论:XRD法可以应用于矿物药生、煅炉甘石的鉴定及其质量控制。     

Data fusion of Fourier transform infrared spectra and powder X-ray diffraction patterns for pharmaceutical mixtures

Fusing complex data from two disparate sources has been demonstrated to improve the accuracy in quantifying active ingredients in mixtures of pharmaceutical powders. A four-component simplex-centroid design was used to prepare blended powder mixtures of acetaminophen, caffeine, aspirin and ibuprofen. The blends were analyzed by Fourier transform infra-red spectroscopy (FTIR) and powder X-ray diffraction (PXRD). The FTIR and PXRD data were preprocessed and combined using two different data fusion methods: fusion of preprocessed data (FPD) and fusion of principal component scores (FPCS). A partial least square (PLS) model built on the FPD did not improve the root mean square error of prediction. However, a PLS model built on the FPCS yielded better accuracy prediction than PLS models built on individual FTIR and PXRD data sets. The improvement in prediction accuracy of the FPCS may be attributed to the removal of noise and data reduction associated with using PCA as a preprocessing tool. The present approach demonstrates the usefulness of data fusion for the information management of large data sets from disparate sources.