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。     

Carboxylesterase catalyzed 18O-labeling of carboxylic acid and its potential application in LC-MS/MS based quantification of drug metabolites

LC-MS quantification of drug metabolites is sometimes impeded by the availability of internal standards that often requires customized synthesis and/or extensive purification. Although isotopically labeled internal standards are considered ideal for LC-MS/MS based quantification, de novo synthesis using costly isotope-enriched starting materials makes it impractical for early stage of drug discovery. Therefore, quick access to these isotope-enriched compounds without chemical derivatization and purification will greatly facilitate LC-MS/MS based quantification. Herein, we report a novel ¹⁸O-labeling technique using metabolizing enzyme carboxylesterase (CES) and its potential application in metabolites quantification study. Substrates of CES typically undergo a two-step oxygen exchange with H₂¹⁸O in the presence of the enzyme, generating singly- and doubly-¹⁸O-labeled carboxylic acids; however, unexpected hydrolytic behavior was observed for three of the test compounds – indomethacin, piperacillin and clopidogrel. These unusual observations led to the discovery of several novel hydrolytic mechanisms. Finally, when used as internal standard for LC-MS/MS based quantification, these in situ labeled compounds generated accurate quantitation comparable to the conventional standard curve method. The preliminary results suggest that this method has potential to eliminate laborious chemical synthesis of isotope-labeled internal standards for carboxylic acid-containing compounds, and can be developed to facilitate quantitative analysis in early-stage drug discovery.     

Circular dichroism detection in high-performance liquid chromatography: Evaluation of the anisotropy factor

The application of a circular dichroism (c.d.) detection system in HPLC using a chiral stationary phase is presented. The simultaneous measurement of the absorbance and c.d. signal allows the evaluation of the anisotropy factor (g = Δ/) and thus the determination of the enantiomeric excess (e.e.) of the eluates. When this detection system is used in preparative chiral chromatography the collection of the enantiomeric fractions can be readily optimized.     

大鼠脑组织单胺类递质及其代谢产物的检测方法研究

目的 :研究大鼠脑组织中单胺类递质及其代谢产物的高效液相反相离子对色谱测定法。方法 :采用LiChrosorbC18,10 μm色谱柱 ,流动相为甲醇 :水 (4 0 :60 ) ,含 0 .0 2 8g LEDTANa2 ,0 .15g LSDS ,0 .2ml LH2 SO4(pH 2 .5～ 3 ) ,荧光检测波长 :λEX=2 85 ,λEM=3 3 3。结果 :对 87只大鼠脑组织中 4种单胺类递质及其代谢产物的含量进行了同时测定 ,高香草酸 (HVA) 2 .5 0～ 40 .0 μg ml、去甲肾上腺素 (NE) 0 .0 1～ 0 .5 0 μg ml、多巴胺 (DA)0 .0 5～ 1.0 0 μg ml、5 羟色胺 (5 HT) 0 .0 2 5～ 0 .5 0 μg ml,峰面积与其含量呈良好的线性关系。 结论 :该法操作简便、快速、准确 ,为组织中单胺类递质及其代谢产物检测的一种理想方法 ,并适用于临床相关研究。     

两种石油加工残油对制备可纺丝中间相沥青的影响

用常压液相炭化法制备中间相沥青，并用熔融法检验中间相沥青的可纺性，研究了汽油裂解残油和催化裂化重柴油参混比的不同对中间相沥青的制备速率，产率，中间相含量，显微结构以及可纺性的影响，指出最佳配比。     

Comparison of assays for determination of peptide content for lyophilized thymalfasin*

Abstract: Precise determination of the peptide content in drug substance samples depends highly upon the particular peptide compound and methodology used. Four independent methods were evaluated and compared to determine which would produce the best experimental precision for analysis of thymalfasin (thymosin α‐1). Four different methods were evaluated including elemental analysis (CHN), quantitative amino acid analysis (AAA), high‐performance liquid chromatography (HPLC), and Kjeldahl. This study demonstrates that the AAA method is highly variable in one laboratory while quite precise in another laboratory. Similarly, HPLC results depended on the laboratory conducting the study with more precise values obtained under cGMP. On the contrary, the CHN method yielded highly precise [i.e. <2% coefficient of variation (CV)] values. As precise knowledge of protein content is fundamental for the compounding of final pharmaceutical product of a specific potency, the CHN analysis is recommended for peptide content determination of the drug substance thymalfasin.     

无国界医生在救援中备灾的重要性

无国界医生致力于应对天灾和战祸所引起的人道医疗危机。灾后实时爆发的人道医疗危机包括急性的外科创伤问题和基础医疗系统的破坏导致疫症发生。本文介绍了无国界医生的救援经验以及专业的备灾体系。     

NIKKISO DBB-27型血液透析机液路系统工作原理及故障报警分析

分析了NIKKISO DBB-27型血液透析机液路系统的系统结构及各组成部分的工作原理,并对相关故障报警的诊断和排除进行了详细论述,为及时、准确地诊断和排除血液透析机的故障提供了理论基础。     

左旋布比卡因复合舒芬太尼或芬太尼在分娩硬膜外自控镇痛的应用

目的探讨左旋布比卡因复合舒芬太尼硬膜外自控镇痛（PCEA）用于分娩镇痛的临床效果及安全性。方法随机选择120例美国标准协会（ASA）I-Ⅱ级初产妇，随机分为舒芬太尼组（A组）、芬太尼组（B组）、无镇痛组（C组），每组40例。A组和B组采用PCEA，C组不给予镇痛药物。观察各组不同时段视觉模拟评分（VAS）和不良反应的发生，同时记录3组产程时间、分娩方式、缩宫使用情况、产后出血量、新生儿Apgar评分。结果A、B2组和C组在PCEA20、60min及宫口开全时VAS差异有统计学意义（P〈0.05）；PCEA5min，A、B2组VAS差异有统计学意义（P〈0.05），2组Bromage评分、不良反应差异无统计学意义（P〉0.05）。3组产程时间、分娩方式、产后出血量、新生儿Apgar评分比较差异均无统计学意义（P〉0.05）。结论左旋布比卡因复合舒芬太尼或芬太尼用于分娩镇痛安全有效，对母婴无明显不良影响。     

HPLC法测定滑膜炎颗粒中原儿茶醛的含量

目的建立滑膜炎颗粒剂中原儿茶醛的含量测定方法质量。方法采用高效液相色谱法对方中原儿茶醛进行含量测定。结果高效液相色谱法测定结果表明原儿茶醛在0．1005～1．005μg范围内呈线性关系，平均加样回收率为99．22％；RSD为0．72％。结论本法简便，重现性好、结果可靠，可作为控制滑膜炎颗粒剂的质量方法。