高效液相色谱法测定血浆中的吉西他滨及其血浆蛋白结合研究

采用高效液相色谱法建立了检测血浆中吉西他滨浓度的方法,并采用平衡透析法测定其血浆蛋白结合率。Aglient ZORBAX SB-C18色谱柱(4.6 mm×250 mm,5μm),流动相为50 mmol/L磷酸氢二钾溶液(p H 3.0±0.1)-甲醇-乙腈(80∶10∶10),检测波长为268 nm,柱温为30℃,流速为1.0 m L/min。吉西他滨在0.2~20.0μg/m L浓度范围内呈现良好的线性关系(r2=0.995 6)。吉西他滨不同浓度在血浆中的蛋白结合率分别为(13.27±2.48)%,(12.64±5.49)%和(14.97±3.97)%。该方法对吉西他滨进行分离,方法简便、灵敏、稳定,其血浆中的血浆蛋白结合率较低。     

RP-HPLC法测定血浆中奥卡西平及其活性代谢物浓度

目的:建立同时测定人血浆中奥卡西平(OXC)及其活性代谢物10,11-二氢-10-羟基卡马西平浓度的实验方法。方法:以阿普唑仑为内标,血浆样本采用甲基叔丁基醚萃取,以RP-HPLC测定,使用Kromasil ~(TM) C18(150 mm×4.6 mm,5μm)色谱柱,流动相为CH3CN-H2O(45︰55,V/V),流速1.0 m L/min,检测波长220 nm,柱温40℃,灵敏度为0.01AUFS。结果:OXC、MHD血浆浓度分别在0.70～11.2μg/m L、2.40～38.40μg/m L范围内线性关系良好,最低检测限分别为0.35μg/m L、1.20μg/m L;两者低、中、高浓度方法平均回收率分别为83.23%～103.17%、87.99%～116.07%;日内RSD(n=3)、日间RSD(n=5)均低于10%。结论:该方法灵敏、准确、简便、快速,可用于OXC与MHD的临床治疗药物监测(TDM)与药动学研究。     

HPLC-UV法测定卡培他滨中的对甲苯磺酸酯

建立了高效液相色谱法测定卡培他滨原料药中的基因毒性杂质对甲苯磺酸甲酯(MepTS)、对甲苯磺酸乙酯(Etp TS)和对甲苯磺酸异丙酯(iPrpTS)。采用C_(18)色谱柱(250 mm×4.6 mm,5μm),紫外检测器在225 nm下直接进样测定。三种对甲苯磺酸酯在0.015～0.15μg/m L浓度范围内线性关系良好,定量限均为0.015μg/m L,检测限均为0.005μg/m L,平均回收率在89.2%～100.3%。该方法简单、准确、专属性强且重现性好,适用于卡培他滨中对甲苯磺酸酯基因毒性杂质的测定。     

RP-HPLC法测定奥利司他原料药的含量

建立奥利司他原料药的含量测定方法。采用高效液相色谱法,Agilent SB-C18色谱柱(25cm×4.6mm,5μm),流动相为甲醇∶水(90∶10);柱温为30℃;流速1.0m L·min-1;进样量20μL。紫外检测器,检测波长为190 nm。主成分奥利司他在0.4~0.6 mg/m L浓度范围内线性关系良好,相关系数r0.999,在相对浓度80%、100%、120%范围内的平均回收率较高。该检测方法精密度及准确度较高,可订入奥利司他原料药的质量标准中,作为含量测定的控制方法。     

紫杉醇纳米脂质载体包封率的测定

建立紫杉醇纳米脂质载体包封率测定的高效液相色谱法。选择色谱条件:Diamonsil-C18柱(200mm×4.6 mm,5μm);柱温30℃;流动相:0.067 mol/L磷酸二氢铵水溶液(三乙胺调p H为7.5)-乙腈(3∶2);检测波长205 nm;体积流量1.0 m L/min;进样量20μL。对该色谱条件下测定紫杉醇的方法学进行考察,建立超滤离心法测定紫杉醇纳米脂质载体的包封率。在此色谱条件下紫杉醇与辅料及溶剂峰均得到良好分离,紫杉醇在50.00~1000μg/m L浓度范围内线性关系良好(R=0.9995,n=7),超滤离心法测得紫杉醇纳米脂质载体的包封率为(88.7±0.2)%。该方法准确可靠、简单快速。可用于紫杉醇纳米脂质载体包封率的测定。     

HPLC-MS/MS法检测2-氯-2-脱氧-D-葡萄糖方法优化及验证

建立了高效液相色谱-三重四极杆串联质谱(HPLC-MS/MS)检测2-氯-2-脱氧-D-葡萄糖(ClDG)的分析方法。采用多反应监测(MRM)负离子电喷雾模式进行HPLC-MS/MS分析。色谱柱为:Alltima Amino 100A 5μm柱(250 mm×4.6 mm),流动相为:V(5 mmol/L乙酸铵)∶V(乙腈)=10∶90;柱温:35℃;流速:1 mL/min;进样量:5μL。ClDG浓度在0.5~37.5μg/m L范围内与峰面积有良好的线性关系,检出限为0.15μg/mL,定量限为0.5μg/mL,方法回收率为92.6%~105.1%。该方法选择性、重复性良好,灵敏度高,能用于ClDG的痕量分析。     

RP-HPLC测定大鼠血浆中土大黄苷的浓度

目的采用RP-HPLC法测定大鼠血浆中的土大黄苷,并进行土大黄苷药代动力学初步研究。方法采用Kromasil C18色谱柱(250mm×4.6 mm,5μm);流动相乙腈-0.5%甲酸水溶液(25︰75);流速1.0 m L·min~(-1);柱温35℃,进样量20μL;检测波长303 nm的色谱条件,医染料木素为内标物,血浆样品采用三氯乙酸去蛋白处理。结果土大黄苷在0.0927~18.530μg·m L~(-1)的范围内与峰面积比值呈现良好线性关系(r=0.9997);最低检测浓度为0.0927μg·m L~(-1);日内和日间精密度良好,RSD均小于8%,专属性、稳定性良好,低温冻融,室温放置均不影响测定结果;回收率为88.94%~92.17%。结论该方法简单、快速、经济、重复性良好,适用于土大黄苷的药代动力学研究。     

高效液相色谱测定鸡肝中洛克沙砷的方法研究

建立了高效液相色谱(HPLC)测定鸡肝中洛克沙砷含量的实验方法。样品经匀浆、甲醇提取、高氯酸去蛋白后,用Nova-Pa k色谱柱(C18,150×3.9 mm,4μm)分离,以0.05 mol/L磷酸二氢钾∶甲醇∶10%乙酸(80∶10∶10)为流动相,在流速0.8 mL/m in,柱温30℃,进样量10μL的条件下,于264 nm波长处检测。结果表明,该方法的线性范围为0.50~10.0μg/mL,线性相关系数R2=0.9741,在两个添加浓度水平上的平均加标回收率分别为83.7%、89.9%。     

高效液相色谱-二极管阵列检测器测定独一味胶囊中木犀草素含量的研究

建立了一种高效液相色谱-二极管阵列检测器(HPLC-DAD)的方法检测独一味胶囊中的木犀草素的含量;采用色谱柱为BDS HYPERSIL C18柱(4.6 mm×250 mm, 5μm),流动相为甲醇-质量分数为0.1%磷酸水溶液(50∶50,V∶V),流速为1.0 mL/min,柱温为35℃;检测波长为350 nm;木犀草素质量浓度在0.1～100μmol/L范围内呈良好的线性关系,在1.0,5.0和10μmol/L三个标准溶液浓度下加标实验,该方法的回收率为97.67%～105.77%,相对标准偏差(RSD)均小于3%,测得独一味胶囊中木犀草素的平均含量为27.4μmol/L;该方法方便可行,灵敏度高,稳定性好,可用于独一味胶囊中木犀草素的含量测定及质量控制。     

HILIC-MS/MS测定牛奶中4种含氮化合物的含量

建立同时检测三聚氰胺、三聚氰酸、尿酸、二氰二胺含量的高效液相-质谱联用方法。采用亲水色谱-串联质谱方法,色谱柱为Agilent Hilic柱(4. 6 mm×100 mm,3. 5μm),以乙腈-水(1∶1)为流动相进行恒度洗脱,流速为1 m L/min,进样量10μL,柱温为25℃。结果三聚氰胺在浓度范围0. 5～20 ng/m L、三聚氰酸、二氰二胺、尿酸的浓度范围均在100～4000 ng/m L内线性关系良好(R≤0. 9986),加样回收率均在82. 5%～115. 0%之间。本方法简便、快速、灵敏度高,适于同时测定牛奶中三聚氰胺、二氰二胺、三聚氰酸、尿酸的含量。     

在线等离子处理

德国NewMaterialsFurth公司正在研究多种材料注射成型期间的在线等离子处理以改进材料的粘合性。该公司在机器人上装有等离子源的Krauss-Maffei2C制造元件KM125-390-160CZ。伴随模具敞开,机器人在接近模制件处使等离子源定位。可准确操纵等离子射束,来处理复杂的几何形状或受限区域。该处理工艺可除去制件表面的污染物,制造出反应性和活性基团,熔化不易粘合的表面层。事实表明,等离子射束可在环境温度条件下操作,该工艺作为非破坏性预处理工艺既有吸引力,也非常有效。NMF公司看到了在线等离子处理的很多应用,例如在金属和薄膜的包胶或…     

Influence of plasma duty cycle during plasma polymerization in adhesive bonding

Junctions between aluminium substrates and ethylene-co-propylene-co-diene terpolymer (EPDM) have been strengthened by depositing alkene functionalized plasma polymers on the aluminium side. The double bonds in the plasma polymer layer were able to covalently bond to the EPDM during the crosslinking step with peroxide. Variations in the peel strength were observed by varying of the plasma duty cycle during plasma polymer deposition. The higher peel strength was obtained with low duty cycles. Analysis of the failure after peel tests showed a cohesive rupture in the EPDM substrate. The differences were explained by analysing the respective concentration of alkene groups in the plasma polymer layer.     

Voltage distribution over capacitively coupled plasma electrode for atmospheric-pressure plasma generation

When capacitively coupled plasma (CCP) is used to generate large-area plasma, the standing wave effect becomes significant, which results in the hindering of the uniform plasma process such as in a plasma etcher or plasma chemical vapor deposition. In this study, the transmission line modeling method is applied to calculate the voltage distribution over atmospheric-pressure CCP electrodes with the size of 1 m × 0.2 m. The measured plasma impedance in our previous study was used in the present calculation. The results of the calculations clearly showed the effects of excitation frequency and the impedance of the plasma on the form of the voltage distribution caused by the standing wave effect. In the case of 150 MHz frequency, the standing wave effect causes a drastic change in the voltage distribution via plasma ignition; however, the change is small for 13.56 MHz. It was also clarified that the power application position is important for obtaining a uniform voltage distribution.     

Photoresist development by plasma

Over the past several years the semiconductor industry has placed major efforts into replacing wet processes with dry processes in fabricating electronic devices. Plasma photoresist stripping, plasma cleaning, and other dry etching techniques have replaced wet methods in many product lines. One area that has received little mention but which is vital toward achieving a totally dry manufacturing process is the dry development of photoresist. One production applicable plasma developable photoresist (PDF) process, using a proprietary resist formulation, is reported. Plasma process characterization, such as end point detection, development latitude, and mechanism are discussed. Included also are development temperature, batch film uniformity, and resolution currently obtainable with the PDF process.     

Steady current plasma macro-nanotechnologies

The paper presents mathematical models and experimental results concerning limited heating with plasma arc of semi-finished products with hard crust in view of their roughing by splintering, extracting of iron from ilmenitic deposits by the plasma jet procedure and production of nanoparticles by thermal decomposition of iron pentacarbonile in the argon plasma jet.     

低温等离子体清洗设备

简要介绍了低温等离子体清洗设备清洗机理、特点及其应用。     

Ball lightning plasma and plasma arc formation during the microwave heating of carbons

Microwave heating can be used to promote heterogeneous reactions with carbon materials, mainly because of the heating mechanism involved in microwave radiation and the phenomenon known as microplasmas. This work presents photographic evidence of plasma formation when different carbon materials are subjected to microwave heating. Two different kinds of plasmas were observed: ball lightning and arc discharge plasmas. The intensity of the plasmas in the less ordered carbon was significantly higher at the beginning of the process.     

Densification of plasma sprayed YSZ electrolytes by spark plasma sintering (SPS)

Solid oxide fuel cells (SOFC) are promising candidates for alternative power generation systems due to their high-energy conversion efficiencies, and low emissions of environmentally hazardous by-products. Plasma spray (PS) is an effective, and relatively inexpensive process for fabricating high performance yttria stabilized zirconia (YSZ) electrolyte for SOFC. Yet, because of the numerous inter-granular defects introduced to the electrolyte by the plasma spray process, the electrolyte is not gas tight and consequently, the energy efficiency of the cell is severely curtailed. In order to improve the performance of the SOFC, spark plasma sintering (SPS) is introduced as a post-spray treatment to enhance the density of the PS YSZ electrolyte rapidly, and effectively. In this study, spark plasma sintering (SPS) was performed at 1200, 1400 and 1500 °C. Each sintering cycle had a holding time of 3 min. Single and multiple SPS cycles (3 min at preset temperature per cycle) were used to treat the plasma sprayed yttria stabilized zirconia (PS YSZ) electrolytes. The microstructure of as-received and SPS treated electrolytes as examined by scanning electron microscopy (SEM) demonstrated a microstructure transition above 1200 °C, where the typical plasma sprayed lamella structure transformed to a granular-type structure. The porosity of as-received and SPS post-treated electrolytes, which were determined by a mercury intrusion porosimeter (MIP) revealed a significant reduction in pores at 1500 °C. Average pore size reduced from 0.2 to 0.08 μm. The ionic conductivity of the electrolytes is evaluated by AC impedance spectroscopy to characterize the effect of SPS on enhancing the ionic conductivity of the electrolytes.