Impurity profiling and in-process testing of drugs for injection by fast liquid chromatography

Liquid chromatography (LC) is considered by many as a mature technique. Nonetheless, LC technology continues to evolve driven by the need for high-throughput and high-resolution analyses. Over the past...     

液相合成β-NaLuF4:Yb3+,Er3+胶体颗粒与光学性质研究

在乙醇—水—油酸—油酸钠液相混合体系中,采用水热合成法制备了油溶性β-NaLuF4:Yb3+,Er3+胶体粒子.用X射线粉末衍射技术测定了样品的物相,结果显示,样品为纯六方相.通过透射电子显微镜和高分辨透射电子显微镜观察到样品两端为六边形纳米棒状或六棱柱状,平均尺寸为10 nm×10 nm ×40 nm.用980 nm半导体激光二极管为激发光源,测定了样品的室温上转换发射谱.结果表明,样品在543 nm处出现强发射峰,对应辐射为Er3+离子从激发态4S3/2至基态4I15/2的跃迁,并通过机理分析确定发光跃迁为双光子发射.     

反相高效液相色谱法测定染毒漆板中马拉硫磷残留量

采用反相高效液相色谱法测定染毒漆板上马拉硫磷残留量。本研究方法以ODS-C18柱（250mm×4.6mm）作为色谱分离柱,80%甲醇：20%水（V/V）为流动相,流速为1.0ml/min,检测波长为220nm的紫外检测器。研究结果表明,在10-100mg/L浓度范围内峰面积与进样量呈良好的线性关系,相关系数r=0.9999;检出限为6.5μg/L（S/N=3）;相对标准偏差RSD为1.36%;平均加标回收率在95%以上。     

HPLC法测定阳春滴丸中淫羊藿苷的含量

目的：通过试验摸索阳春滴丸的含量测定控制方法。方法：色谱柱：Hedra ODS-2（Size：250mm×4.6mm,Media：10nm5um）;乙腈：水（25：75）为流动相;流速0.8ml/min。检测波长270nm。结果：淫羊藿苷进样量在0.112~0.560μg之间与峰面积分值呈线性关系（r=0.9998）,平均加样回收率达98.85%。重复性试验RSD%值为0.55%。结论：所建方法可行,专属性、重复性好,可用于阳春滴丸的质量控制。     

Development of the fingerprints for the quality evaluation of Viscum coloratum by high performance liquid chromatograp

A high-performance liquid chromatography coupled ultraviolet （HPLC-UV） method was developed for a chemical fingerprint analysis of Viscum coloratura. Eighteen peaks were selected as the common peaks and Homoeriodictyol-7-O-β-D-apiosiyl-（1→2）-β-D-glucoside     

陶瓷—金属活性金属钎焊研究的现状和进展

在现有的陶瓷-金属连接技术中，活性金属钎焊具有显著的技术优势和经济效益。本文综述了近年来在反应浸润、活性钎料、界面反应、连接强度和部分瞬间液相连接方面的研究现状和进展，指出了有待进一步研究的问题。     

Quantitative analysis of a novel antimicrobial peptide in rat plasma by ultra performance liquid chromatography-tandem mass spectrometry

We described the first results of a quantitative ultra performance liquid chromatographytandem mass spectrometry method for a novel antimicrobial peptide （phylloseptin, PSN-1）. Chromatographic separation was accomplished on a Waters bridged ethyl hybrid （BEH） C18 （50mm× 2.1 mm, 1.7 μm） column with acetonitrile-water （25：75, v/v） as isocratic mobile phase. Mass spectrometry detection was performed in the positive electrospray ionization mode and by monitoring of the transitions at m/z 679.6/120, 509.6/120 （PSN-1） and m/z 340.7/165 （Thymopentin, IS）. Protein precipitation was investigated and the recovery was satisfactory （above 82%）. The method was shown to be reproducible and reliable with intra-day precision below 5.3%, inter-day precision below 14.2%, and linear range from 0.02 to 2 lag/mL with r〉0.994. The method was successfully applied to a pharmacokinetic study of PSN-1 in rats after intravenous administration.     

对硝基苯磺酰甲基苯及其衍生物与甲基丙烯酸酯的加成重排羰基化反应

在固—液相转移催化剂作用下，对硝基苯磺酰甲基苯及其衍生物与甲基丙烯酸酯反应，得到连续Michael加成重排羰基化产物．产物的结构特征都已通过质谱(MS)、红外光谱(IR)、^1HNMR谱和元素分析得到表征．同时提出了一个可能的反应机理．     

气相色谱法测定潜艇空气中甲苯和二甲苯的代谢物

本文提出了一种测定尿中马尿酸和甲基马尿本的气相色谱法。该方法的精密度为ＨＡ：１．６％－１．９％；ＭＨＡ：１．８％－２．８％，准确度为ＨＡ：９５．０％－１０３．％，ＭＨＡ：９６．７％－１０５．０％，ＨＡ和ＭＨＱ的最低检出浓度均为１．０ｍｇ／Ｌ，尿样加入１％的氯仿在４℃下可保存４０天以上。