Facile Synthesis of Enantiomerically Pure 1-（5-Bromo-2-chlorophenyl）-1-（4-ethoxyphenyl）ethane

A facile 7-step procedure for the synthesis of enantiomerically pure 1-（5-bromo-2-chlorophenyl）-1-（4-ethoxyphenyl）ethanes[（R）-2 and（S）-2] that started from （5-bromo-2-chlorophenyl）（4-ethoxyphenyl）methanone 3 was developed.The key step was the resolution of 2-（5-bromo-2-chlorophenyl）-2-（4-ethoxyphenyl）acetic acid 6 by crystallizations of its L-and D-menthyl esters 7 and 8 from petroleum ether to give optically pure enantiomers 9 and 10,respectively.The absolute configurations of the products were unambiguously determined by single-crystal X-ray diffractions of four key intermediates,9,10,13 and 14.This procedure is characterized by inexpensiveness,scalability and ability to produce two individual enantiomers of a diarylethane with unambiguously determined absolute configurations and high enantiomeric purities.     

基于中阶梯光栅光谱仪的激光诱导等离子体分析系统研究

为了满足激光诱导等离子体分析系统(LIPS)对分光系统的分辨率,光谱范围,体积等多方面要求。本文研制了一台中阶梯光栅光谱仪,该光谱仪能同时获得所有谱段范围内的光谱信息,令LIPS系统可实现快速在线实时分析。并且,该光谱仪采用可调节延迟时间的ICCD作为后端探测器,令整个系统可根据实际实验情况选择最优延迟时间接收光谱,提高了整个系统的信噪比。最后,搭建了一套激光诱导等离子体分析系统,对研制的中阶梯光栅光谱仪在系统中的可用性进行验证。通过对合金样品测试,整个系统的分辨率达0.02 nm,光谱范围覆盖190～600 nm。并且研制的LIPS系统光谱重复性较好,特征元素波长提取误差不超过0.01 nm,可较准确的对样品成分进行分析。     

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利用一套四极质谱气体分析与测试系统,开展MicroVision Plus四极质谱计的氦(He)、氘(D2)分辨性能实验。分别向分析室送入He和D2,记录质谱图,得到质量刻度和分辨率等信息。He+峰位为(4.0022±0.0006)amu;D2+峰位为(4.0246±0.0006)amu。在10-6～10-4Pa的分压范围,观察到He和D2的分辨率随其分压强的增大而减小。在10-7Pa-m3-s-1的He漏孔条件下,调节D2送气量,He+/D2+分压峰值比在10-1量级可以分辨出He。     

Development and Validation of Rapid Resolution RP-HPLC Method for Simultaneous Determination of Atorvastatin and Related Compounds by Use of Chemometrics

Abstract

A Rapid Resolution Reversed Phase High-Performance Liquid Chromatography (RR RP-HPLC) method has been developed and validated for the simultaneous determination of atorvastatin and seven related compounds specified as impurities. Experimental design was used during method optimization (full factorial 3² design) and robustness testing (central composite design). Chromatography was performed with mobile phase containing phosphate buffer pH 3.5 and a mixture of 10% (v/v) tetrahydrofuran in acetonitrile as organic modifier. A Zorbax Eclipse XDB C18 Rapid Resolution HT 4.6 mm × 50 mm, 1.8 µm particle size column was used. The developed method allowed determination of Atorvastatin Calcium (ATV Ca) purity and level of impurities in drug substances.     

宽光谱Czerny-Turner光谱仪中的彗差与分辨率

小型光谱仪较多地采用Czerny-Turner(切尼—特纳)光路结构,其设计应遵循Shafer消彗差原理消除中心波长处的初级彗差并尽量平直整个谱面以提高分辨率。但常规设计并未考虑非中心波长处彗差和分辨率的变化情况。在对两种典型切尼—特纳光路结构进行初级彗差分析的基础上,指出交叉型光路结构宽光谱范围内的分辨率呈“V”形,而M型光路结构分辨率在全光谱范围内变化较小,近似呈“一”形,即后者宽光谱范围内的分辨率一致性远好于前者。针对于此,该文设计了光谱范围为400～600 nm的2种光路,并对其进行了理论计算和对比实验,实验结果表明,两者边缘波长处分辨率分别比中心波长处分辨率低3.7倍和1.2倍,与理论计算结果基本一致。     

LINEAR ISOMETRIC NON-ANTICIPATIVE TRANSFORMATIONS OF WIENER PROCESS

ThispaperisanoutcomeofnumerousdiscusionsandexchangeofideaswithlatePredragPerunicic,whosedeepandprofoundmathematicalknowledgeandhumanvaluesgaveusaninspirationandmotivationtofinalizeourjointideas.1.Wereferto[3,4]forthenotionofspectralmultiplicitytheoryintheseparableHilbertspace.LetHbeacyclicHilbertspacewiththeresolutionoftheidentity{p(t)}ofthemaximalspectraltypelIP(dt)ll'~dt-ordinaryLebesguemeasure.Anon-anticipativelineartransformationsisdefinedbyVolterrakernelg(t,u),uSt,ajsf'g(t)u)p(du),t>0…     

Crystallization of benzimidazole by solution growth method and its characterization

The potential organic NLO crystal of benzimidazole (BMZ) has been successfully grown by slow evaporation solution growth technique at room temperature. The crystalline perfection has been verified by High resolution X‐ray diffraction (HRXRD) analysis. The very low angle boundary obtained for this solution‐grown specimen may be attributed to the segregation of solvent molecules (methanol), which were entrapped within the crystal during growth. The laser damage threshold has been measured by using high intensity Q‐switched Nd:YAG laser. The observed value is greater than that of KDP and lesser than that of melt grown benzimidazole. The NLO efficiency has been determined and it is compared with the KDP crystal. The thermal behaviour has been assessed by TG/DTA analysis. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

二维小波变换与子窗口因子分析法结合用于含噪声HPLC-DAD数据的解析

将二维小波变换与子窗口因子分析法相结合,用于模拟的高噪声HPLC-DAD数据的解析.首先应用二维小波变换滤除噪声,然后采用子窗口因子分析法解析重叠峰.结果表明,信噪比为10的高噪声基本被滤除掉.