不同规格怀牛膝不同极性部位HPLC指纹图谱

目的研究并比较不同规格怀牛膝不同极性部位的HPLC指纹图谱,探索其内部质量差异,为该药材的规格标准完善及临床用药提供参考。方法将怀牛膝用体积分数75%乙醇水浴回流提取,得体积分数75%乙醇回流提取物,用40 mL水溶解后,依次用石油醚、三氯甲烷、乙酸乙酯、正丁醇进行萃取,得到各萃取相及萃取后的水相,浓缩至浸膏,采集各部位HPLC指纹图谱;运用相似度、综合聚类法进行数据分析,同时对其不同部位的指纹图谱进行比对分析。结果石油醚、氯仿部位均标定了11个共有峰,乙酸乙酯部位标定了10个共有峰,正丁醇部位标定了19个共有峰,水部位标定8个共有峰;氯仿部位指纹图谱相似度差异较大,其他部位指纹图谱相似度差异较小,均在0.9以上;石油醚部位指纹图谱差异主要体现在峰高,乙酸乙酯部位、氯仿部位、水部位的化学成分种类及峰高均存在差异;综合聚类分析能将不同规格怀牛膝区分开。结论不同规格怀牛膝内部质量存在差异;实验中所建立的HPLC指纹图谱可以全面反映不同规格怀牛膝的化学成分分布,为不同规格怀牛膝的整体质量评价提供参考。     

Quantitative chemical exchange saturation transfer (qCEST) MRI – omega plot analysis of RF‐spillover‐corrected inverse CEST ratio asymmetry for simultaneous determination of labile proton ratio and exchange rate

Chemical exchange saturation transfer (CEST) MRI is sensitive to labile proton concentration and exchange rate, thus allowing measurement of dilute CEST agent and microenvironmental properties. However, CEST measurement depends not only on the CEST agent properties but also on the experimental conditions. Quantitative CEST (qCEST) analysis has been proposed to address the limitation of the commonly used simplistic CEST‐weighted calculation. Recent research has shown that the concomitant direct RF saturation (spillover) effect can be corrected using an inverse CEST ratio calculation. We postulated that a simplified qCEST analysis is feasible with omega plot analysis of the inverse CEST asymmetry calculation. Specifically, simulations showed that the numerically derived labile proton ratio and exchange rate were in good agreement with input values. In addition, the qCEST analysis was confirmed experimentally in a phantom with concurrent variation in CEST agent concentration and pH. Also, we demonstrated that the derived labile proton ratio increased linearly with creatine concentration (P < 0.01) while the pH‐dependent exchange rate followed a dominantly base‐catalyzed exchange relationship (P < 0.01). In summary, our study verified that a simplified qCEST analysis can simultaneously determine labile proton ratio and exchange rate in a relatively complex in vitro CEST system. Copyright © 2015 John Wiley & Sons, Ltd.     

水分去除的方法及其在药物合成中的应用

化学药合成过程中水分残留不利于反应的进行,还影响药物及制剂的稳定性、理化性质、溶出及药理作用等,因此水分几乎是大多数药物合成中的必测项目,通过有效除水严格控制反应体系中水分的含量至关重要。本文综述了水分的存在形式,常见除水剂和脱水剂的种类、作用原理与除水能力,以及在药物合成的应用,为药物合成反应中水分的去除提供参考。     

Fast CT-PRESS-based spiral chemical shift imaging at 3 Tesla.

A new sequence is presented that combines constant-time point-resolved spectroscopy (CT-PRESS) with fast spiral chemical shift imaging. It allows the acquisition of multivoxel spectra without line splitting with a minimum total measurement time of less than 5 min for a field of view of 24 cm and a nominal 1.5x1.5-cm2 in-plane resolution. Measurements were performed with 17 CS encoding steps in t1 (Deltat1=12.8 ms) and an average echo time of 151 ms, which was determined by simulating the CT-PRESS experiment for the spin systems of glutamate (Glu) and myo-inositol (mI). Signals from N-acetyl-aspartate, total creatine, choline-containing compounds (Cho), Glu, and mI were detected in a healthy volunteer with no or only minor baseline distortions within 14 min on a 3 T MR scanner.     

C60的化学反应性和高分子化

综述了C_(60)化学研究的进展。C_(60)的化学反应性的研究展现了一个广阔的新领域,并使C_(60)作为一种新型的功能基团引入高分子成为现实。这些进展为进一步深入研究C_(60)尤其是C_(60)的材料化提供了前提。     

尼罗罗非鱼肉营养成分分析

<正> 尼罗罗非鱼(Tilapia nilotica)是我国从非洲引进的热带鱼类,具有刺少肉味鲜嫩、食性广、生长快、繁殖力强、养殖周期短等特点。已快速地养殖到全国各地。作者对利用地热资源人工喂养条件下的尼罗罗非鱼肉的氨基酸和肉内的粗蛋白、脂肪、维生素等成分进行分析,评估尼罗罗非鱼肉的营养价值,从营养学的角度为人们提供科学依据。     

仡佬族成人指纹白线的研究

目的　探讨仡佬族成人指纹白线的特征 ,为法医学、人类学及临床医学提供参考资料。方法　对贵州省道真县三代均为仡佬族的 2 17名成年人的 43 4侧手、2 170个手指指纹白线出现率进行了观测和统计分析。结果　各指指纹白线出现率为 :男 2 .48% ,女 2 .76% ;每个人指纹白线出现率 (每人有一指以上出现者 )为 :男 17.82 % ,女 18.10 % ;每只手指纹白线出现率 (每指有一条白线以上出现者 )为 :男 10 .89% ,女 11.2 1% ;每只手指指纹白线分布率为 :男 2 .48% ,女 2 .76% ;男女间差异无显著性 ,P >0 .0 5。结论　仡佬族成年人指纹白线出现率较低 ,并以单手、单指、单条白线分布为主。     

辽宁满族和汉族指纹白线正常值分析

本文报告了辽宁满族和汉族人指纹白线的调查结果。满族和汉族人的指纹白线出现率分别是7.14％和31.73％。满族人的指纹白线出现率低于汉族、维吾尔族、德国人、波兰人和美国白人。作者注意到满族人的指纹白线不存在左右手间和性别间的差异,而汉族人性别间差异显著。十指均有白线频率为1.91％(满族)和10.5％(汉族)。十指均有白线的白线平均数满族为39.3±6.6,汉族为35.5±10.6。五指中指纹白线出现率从高到低的顺序在满族为Ⅰ、Ⅳ、Ⅲ、Ⅱ、Ⅴ,在汉族为Ⅳ、Ⅲ、Ⅱ、Ⅰ、Ⅴ。存在民族间的差异。     

睾丸旁促结缔组织增生性小圆细胞肿瘤1例报告及文献复习

目的:探讨睾丸旁促结缔组织增生性小圆细胞肿瘤的临床、病理特征、诊断及治疗。方法:回顾分析1例睾丸旁促结缔组织增生性小圆细胞肿瘤的诊治及随访资料,并复习相关文献。患者,男,27岁,因阴囊内无痛性肿块4个月就诊。体检于左侧阴囊内可扪及囊性肿块,同侧睾丸不能扪及。行左侧睾丸根治性切除术,术后辅以化疗。结果:术中见左侧睾丸旁多发结节状隆起肿块,质偏硬;术后病理检查肿瘤细胞呈巢状或梁索状结构并埋没在增生的纤维结缔组织中;免疫组化显示瘤细胞具有上皮源性、间质性和神经源性等多向分化的特点。术后已随访3年无瘤生存,预后良好。结论:促结缔组织增生性小圆细胞肿瘤有特异的临床病理特征,好发于年轻男性,手术切除肿瘤联合化疗是治疗的主要方法,睾丸旁促结缔组织增生性小圆细胞肿瘤比腹腔型预后相对好。     

Preparation of protected peptidyl thioester intermediates for native chemical ligation by Nα‐9‐fluorenylmethoxycarbonyl (Fmoc) chemistry: considerations of side‐chain and backbone anchoring strategies,and compatible protection for N‐terminal cysteine*,†

Abstract: Native chemical ligation has proven to be a powerful method for the synthesis of small proteins and the semisynthesis of larger ones. The essential synthetic intermediates, which are C‐terminal peptide thioesters, cannot survive the repetitive piperidine deprotection steps of N^α‐9‐fluorenylmethoxycarbonyl (Fmoc) chemistry. Therefore, peptide scientists who prefer to not use N^α‐t‐butyloxycarbonyl (Boc) chemistry need to adopt more esoteric strategies and tactics in order to integrate ligation approaches with Fmoc chemistry. In the present work, side‐chain and backbone anchoring strategies have been used to prepare the required suitably (partially) protected and/or activated peptide intermediates spanning the length of bovine pancreatic trypsin inhibitor (BPTI). Three separate strategies for managing the critical N‐terminal cysteine residue have been developed: (i) incorporation of N^α‐9‐fluorenylmethoxycarbonyl‐S‐(N‐methyl‐N‐phenylcarbamoyl)sulfenylcysteine [Fmoc‐Cys(Snm)‐OH], allowing creation of an otherwise fully protected resin‐bound intermediate with N‐terminal free Cys; (ii) incorporation of N^α‐9‐fluorenylmethoxycarbonyl‐S‐triphenylmethylcysteine [Fmoc‐Cys(Trt)‐OH], generating a stable Fmoc‐Cys(H)‐peptide upon acidolytic cleavage; and (iii) incorporation of N^α‐t‐butyloxycarbonyl‐S‐fluorenylmethylcysteine [Boc‐Cys(Fm)‐OH], generating a stable H‐Cys(Fm)‐peptide upon cleavage. In separate stages of these strategies, thioesters are established at the C‐termini by selective deprotection and coupling steps carried out while peptides remain bound to the supports. Pilot native chemical ligations were pursued directly on‐resin, as well as in solution after cleavage/purification.