Simultaneous determination of rosiglitazone and metformin in plasma by gradient liquid chromatography with UV detection

A novel, fast and simple liquid chromatographic method was developed and validated for the simultaneous determination of rosiglitazone and metformin in human plasma. The analysis was performed on a phenyl column (250 mm × 4.6 mm i.d., 5 μm) using a gradient method starting with mobile phase composed of acetonitrile:5 mM acetate buffer pH 5.5 (75:25, v/v). The flow rate was 1 mL min⁻¹. UV detection was performed at 245 nm and verapamil was used as internal standard. The total run time was less than 10 min. Sample preparation included a simple protein precipitation step with acetonitrile. Validation experiments were performed to demonstrate stability, specificity, sensitivity, linearity, accuracy, precision and robustness. The limit of quantification was 100 ng mL⁻¹ for rosiglitazone and 250 ng mL⁻¹ for metformin. The extraction recoveries were 100.02-105.0% for rosiglitazone and 105.64-103.88% for metformin. The method was applied with success to plasma samples obtained from diabetic patients undergoing treatment with rosiglitazone and metformin.     

Separation of proteins with a molecular mass difference of 2 kDa utilizing preparative double-inverted gradient polyacrylamide gel electrophoresis under nonreducing conditions: application to the isolation of 24 kDa human growth hormone

A method for separating proteins with a molecular mass difference of 2 kDa using SDS-PAGE under nonreducing conditions is presented. A sample mixture containing several human growth hormone (hGH) isoforms was initially separated on a weak anion-exchange column. Fractions rich in 24 kDa hGH as determined by analytical SDS-PAGE were pooled and further separated by cation-exchange chromatography. The fractions pooled from the cation-exchange chromatography contained two hGH isoforms with a 2 kDa molecular mass difference according to SDS-PAGE analysis, 22 and 24 kDa hGH. The 22 and 24 kDa hGH were separated using continuous-elution preparative double-inverted gradient PAGE (PDG-PAGE) under nonreducing conditions. The preparative electrophoresis gel was composed of three stacked tubular polyacrylamide matrices, a 4% stacking gel, a 13-18% linear gradient gel, and a 15-10% linear inverted gradient gel. Fractions containing purified 24 kDa hGH were pooled and Western blot analysis displayed immunoreactivity to antihGH antibodies. PDG-PAGE provides researchers with an electrophoretic technique to preparatively purify proteins under nonreducing conditions with molecular mass differences of 2 kDa.     

New uniform algorithm to predict reversed phase retention values under different gradient conditions

A new numerical emulation algorithm was established to calculate retention parameters in RP-HPLC with several retention times under different linear or nonlinear binary gradient elution conditions and further predict the retention time under any other binary gradient conditions. A program was written according to this algorithm and nine solutes were used to test the program. The prediction results were excellent. The maximum relative error of predicted retention time was less than 0.45%.     

Topical Problems in Elemental Analysis of Advanced Ceramic Materials

Selected prominent problems in the analysis of advanced ceramic materials are surveyed. The importance of reliability of results is discussed in the field of elemental trace- and microanalysis in view of its interaction with economy, power of detection, local resolution and speciation selectivity. Particular problems in the analysis of major constituents, trace components and microlocal distributions are based on the striking propertics of ceramics; they are exemplified. Analytical assistance must start from the beginning of the production processing, in the preparation of the powdered base materials. Determination of the stoichiometry requires high accuracy and differentiation of chemical species in bulk and surface analysis of ceramic base powders. Element trace determination by direct instrumental methods requires standard reference materials for calibration; these are currently inavailable in a sufficient variety. For optimum reliability and power of detection, element traces must be prepared in isolated form in a small excitation volume for analysis. A review on the state-of-the-art of wet-chemical combined procedures is presented. Decomposition position procedures are emphasized, due to their risk of contributing severe systematic error. Combustion in elementary fluorine is presented for decomposition of refractory materials. The performance of some direct procedures is discussed. Very efficient methods are available for element trace determinations in ceramic materials, offering high detection power. Several approaches for high-resolution local microanalysis in non-conductive ceramic materials are identified as the most promising development in the analysis of sintered compact ceramic products and devices.     

梯度洗脱测定植物源调节剂中内源激素方法探讨

建立了梯度洗脱高效液相色谱法同时测定内源激素赤霉素(GA3)、吲哚乙酸(3-IAA)、脱落酸(ABA)、细胞分裂素(6-BA)和α-萘乙酸(α-NAA)等5种植物内源激素的方法,采用Hypersil ODS C18柱和紫外检测器,以甲醇、乙腈和0.6%的乙酸为流动相梯度洗脱,分别在各组分的保留时间段设置其最佳检测波长,在12 min内可将上述5种内源激素的各组分分离完全,峰形良好,该方法的回收率可达到90%～96%,线性相关系数(r)大于0.998,检出限在0.02～0.3 μg/g之间.还探讨了各组分的最佳检测条件和梯度洗脱存在的问题及解决方法.     

大口径光学元件波前调制PSD模拟分析

 使用PSD作为大口径光学元件表面加工质量的评价参数，针对不同的波前调制进行了初步的模拟计算，得到了不同调制频率和不同调制深度情况下的PSD曲线变化情况。当调制频率不同时，PSD曲线的突变部分会发生相应的频移，调制频率高则突变发生在空间频率较高的频段，同时PSD峰值不变。相对应调制深度不同时，PSD曲线的突变部份峰值发生变化，调制深度大则峰值大，与此同时峰值出现的位置不会发生变化。计算和分析结果表明PSD分析结果能够在频率域反应出元件表面受到的不同程度的调制信息。     

电爆炸箔断路开关的理论和实验研究

 采用金属箔电爆炸过程的二维数值计算模型，对含电爆炸金属箔断路开关的电感储能脉冲功率调节系统进行了数值计算。以此为基础，研制出了一种低电感型的电爆炸箔断路开关，并以4μF/75kV脉冲电容器组作为初级能源，13Ω电阻作为负载进行实验研究。研究结果表明：在负载上可获得约250kV，脉宽大于400ns的脉冲电压。     

强流射频四极加速器输入耦合环的物理设计研究

 详细讨论了强流射频四极加速器高频输入耦合环的一些基本问题，完成了高频输入耦合环的初步物理设计. 利用二维程序Superfish 的一些结果，确定了耦合环的大小，计算了耦合环的功耗，并对构成耦合环导线的粗细进行了估算。该耦合环的物理设计可作为耦合环试验的基础，同时，也可作为三维程序HFSS 模拟计算的起点。     

光谱法锌离子检测系统的研究

采取标准锌显色剂与锌发生显色反应，生成不溶于水的絮状络合物。用光谱仪测它的吸光度，研究其特征谱与吸光度的特点，建立其浓度与特征波长吸光度间的数学模型。本文所采用的显色剂主要与锌、铜、镉、镍四种离子发生络合反应。因此分别探索了四种离子高浓度以及低浓度时显色反应的吸光度，最终通过得到锌离子浓度与吸光度的关系式以及锌离子浓度与四波长下四种离子混合溶液显色后的吸光度的关系式，给出了锌离子的吸光度与总吸光度的关系式。显色反应能否满足分光光度法的要求，主要与显色剂的性质有关，同时显色反应的条件也至关重要。因为在显色反应过程中，主要是锌离子与锌显色剂发生络合反应形成络离子，进而形成絮状络合物。络离子一般比较稳定，但在水溶液中也存在着电离平衡，也就是说当显色条件发生变化时，既有可能形成络离子，也有可能发生络离子的分解，从而影响络合反应的程度。显色条件包括显色剂用量、pH值、反应温度、显色时间、待测溶液的盐度以及浊度等。重点研究待测溶液的盐度对锌离子浓度测量值的影响，并通过实验给出影响规律以及校正模型。