超高效液相色谱三重四极杆质谱联用法快速检测尿液和血浆中鹅膏毒肽和鬼笔毒肽

建立了同时快速检测尿液和血浆中3种鹅膏毒肽和2种鬼笔毒肽的超高效液相色谱三重四极杆质谱联用分析方法。尿液样品直接进样,血浆样品经乙腈沉淀除蛋白后,在UPLCHSST3色谱柱上分离,正离子电喷雾多反应监测(MRM)模式检测,基体匹配标准外标法定量。尿液和血浆样品的线性范围分别为2～100和1～100μg/L;加标回收率分别在92.0%～108.0%和85.0%～100.0%的范围内;相对标准偏差为1.0%～22.0%和2.0%～22.0%(n=6);样品的检出限为0.2～1.0μg/L和0.1～0.5μg/L(S/N=3)。本方法灵敏,简单,快速,特异性强。     

9-芴甲氧羰酰氯柱前衍生-高效毛细管电泳法测定人血浆中牛磺酸

建立了区带毛细管电泳法快速测定人血浆中牛磺酸的方法.血浆样品经乙腈沉淀蛋白并离心后,上清液中牛磺酸与9-芴甲氧羰酰氯在室温及pH 9.5条件下避光反应20 min,生成具有紫外吸收的衍生产物,以40 mmol/L的乙酸钠(pH 4.6)为运行缓冲溶液,熔融石英毛细管为分离柱;分离电压22kV;紫外检测.实验结果表明:在优化的实验条件下,样品检测仅需9 min,牛磺酸质量浓度在2.5~40.0 μg/mL范围内具良好线性关系(r=0.9995),检出限为0.8 mg/L(S/N=3),迁移时间和峰面积RSD分别为0.27%和1.8%,加标回收率90.3%～108.0%.用本法测定18名健康成人血浆中的牛磺酸,均值为15.8±3.2μg/mL.     

亲水液相色谱三重四极杆质谱联用法快速检测尿液和血浆中河豚毒素

建立了快速检测尿液和血浆中河豚毒素的亲水液相色谱三重四极杆质谱联用分析方法.样品经乙腈沉淀、TSK-gel Amide-80亲水色谱柱分离后,采用电喷雾串联质谱多反应监测(MRM)模式检测,基体匹配标准外标法定量.尿液和血浆样品的线性范围分别为3～500 μg/L和1～200 μg/L,加标回收率分别为96%～108%和100%～105%,相对标准偏差小于9%和16%(n=6),样品的检出限分别为1.0和0.3 μg/L(S/N=3).本方法简单、快速、灵敏、特异性强.     

气相色谱法测定溴己新血药浓度及药代动力学研究

 建立了人血浆中溴己新的气相色谱 电子捕获测定法 ,对溴己新胶囊在健康人体内的药代动力学进行了研究。色谱柱为 5 %SE 30 (2m× 3mmi.d .)硅烷化玻璃柱。 5 氯 2 氨基二苯甲酮为内标 ,血浆样品加入磷酸盐缓冲液 (pH 6 0 )后用正己烷 二氯甲烷 (体积比为 9∶1)提取。线性范围为 1 0 μg/L～ 5 0 0 μg/L ,r =0 9994。人血浆中最小检测质量浓度为 0 5 μg/L。方法重现性好 ,日内、日间RSD分别小于 4 5 6 %和 7 11% ,平均回收率 97 5 %。 8名健康志愿者口服 8mg溴己新胶囊后 ,其体内代谢过程符合一房室模型。     

反相高效液相法测定血浆及尿液中的异烟肼

 建立了血浆及尿液中异烟肼的高效液相快速测定方法 ,以满足临床药物分析和法医学鉴定的需要 ,提高对血浆及尿液中异烟肼浓度检测的准确性。以香草醛为衍生化试剂 ,将异烟肼经柱前衍生为异烟肼 香草醛腙 ,直接对处理后样品中的腙进行定性、定量分析。以在空白人体液样本中定量添加标准异烟肼的方法考察了样品的前处理方法、仪器条件、线性范围、精密度、回收率等 ,并对健康受试者血液中的异烟肼浓度进行了监测。结果表明 ,方法的线性范围为 0 2mg/L～ 1 2 0mg/L ;检测限为 0 2mg/L ;日内、日间精度均小于 4 0 % (n =5) ;回收率在96 3 %以上。     

气相色谱法测定溴己新血药浓度及药代动力学研究

建立了人血浆中溴己新的气相色谱 电子捕获测定法 ,对溴己新胶囊在健康人体内的药代动力学进行了研究。色谱柱为 5 %SE 30 (2m× 3mmi.d .)硅烷化玻璃柱。 5 氯 2 氨基二苯甲酮为内标 ,血浆样品加入磷酸盐缓冲液 (pH 6 0 )后用正己烷 二氯甲烷 (体积比为 9∶1)提取。线性范围为 1 0 μg/L～ 5 0 0 μg/L ,r =0 9994。人血浆中最小检测质量浓度为 0 5 μg/L。方法重现性好 ,日内、日间RSD分别小于 4 5 6 %和 7 11% ,平均回收率 97 5 %。 8名健康志愿者口服 8mg溴己新胶囊后 ,其体内代谢过程符合一房室模型。方法可用于体内血药浓度测定 ,简单、快速 ,灵敏度高 ,数据准确可靠     

超高效液相色谱-串联质谱法测定鸡血浆中利巴韦林及其主要代谢物

建立了同时检测血浆中利巴韦林(Ribavirin)及其主要代谢物1H-1,2,4-三氮-3-甲酰胺(TCONH2)和1-β-D-呋喃基核糖-三氮唑-3-羧酸(RTCOOH)的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。鸡血浆样品加入13C5-利巴韦林内标,以甲醇沉淀蛋白,经ZORBAX SB-Aq(100 mm×3 mm,1.8μm)色谱柱分离,以0.1%甲酸水-甲醇为流动相,梯度洗脱,采用正离子多反应监测模式(MRM),内标法定量。结果表明:利巴韦林、TCONH2与RTCOOH的线性范围分别为5~5 000,5~5 000,50~5 000μg/L,相关系数(r2)分别为0.994 7,0.999 2,0.997 6。质控样品的加标回收率为84.1%~108.2%,批内相对标准偏差(RSD,n=6)为1.6%~13.4%,批间RSD(n=12)为3.8%~16.9%。样品的检出限(S/N=3)为2~10μg/L。本方法快速简便,有效排除了内源性干扰,方法的线性范围宽,重复性好,适用于血浆样品中利巴韦林及主要代谢产物的测定。     

氢化物发生-原子荧光光谱法测定植物样品中的硒

本文应用氢化物发生-原子荧光光谱法对植物样品中硒总量的测定方法进行研究。优化了植物样品预处理,选取H2O2-HNO2(1∶5,V/V)体系微波消解;优化了测定中载流与还原剂的浓度,选定载流HCl浓度为15%,还原剂KBH4浓度为1.5%。该方法测定植物样品中的总硒,线性范围为0~100μg/L(r=0.9995),检出限为0.0906μg/L,回收率在90.0%~112.2%范围,精密度(RSD)小于0.39%。该方法操作简单、灵敏度高、检出限低,适合对植物样品中硒总量的分析测定。     

凝血酶时间法测定家兔血浆中重组水蛭素

建立了凝血酶时间(thromb in tim e,TT)法测定国产重组水蛭素血药浓度的方法,以便为进一步研究该药在家兔体内的药物代谢动力学提供方法学基础。重组水蛭素血浆水平依其抗凝血酶活性(TT延长)予以测定。对该法的影响因素进行了探讨,最适测定条件确定为5 U/mL的凝血酶溶液,0.1 mol/L pH 7.4的Tris-HCL缓冲液及血浆各50μL;结果发现对凝血酶时间延长百分率的对数与浓度呈线性相关,r为0.98~0.99;线性范围为0.12~0.60 mg/L,定量限为0.12 mg/L。日内和日间精密度(RSD)分别为5.6%~9.1%和9.2%~11.5%;方法回收率97.5%~99.2%;超出线性范围的高浓度血浆样品作2~100倍稀释,其稀释回收率为92.4%~94.8%。血浆样品在-20℃冰冻保存,至少1星期内稳定。应用本方法测定家兔iv重组水蛭素2.0 mg/kg后不同时间血药浓度,表明该药符合二室模型、一级动力学过程。     

气相色谱/质谱测定汽油中的元素硫

在气相色谱/质谱(GC/MS)联用仪上,研究了汽油中元素硫存在的结构,并采用外标法定量,开发出了汽油中元素硫测定的新方法。样品直接进样(进样量1 μL),完成一个样品分析只需16 min,最小检测量(MDQ)为9.55 pg。与现有的其他元素硫分析方法相比,该方法更简便 快速 灵敏,且无干扰。该方法选择了最佳分析条件,因而线性范围宽(0.01-100 mg/L),线性相关系数大于0.9995;方法精确度高,元素硫检测的相对标准偏差(RSD)＜5%,回收率为93.01%-106.21%。该方法样品用量少     

等离子体聚合及其聚合物的应用

本文着重综述了烃,含氮、氧的有机化合物,碳氟化合物以及有机硅化合物的等离子体聚合。同时还系统地介绍了等离子体聚合物在制备反渗透膜、分离膜、材料表面的涂层等方面的国内外的最新研究成果。     

等离子体聚合法

扼要介绍等离子体聚合的原理、设备和方法,对其应用也作了叙述。     

Plasma medicine

Different aspects of plasma medicine, the new branch interdisciplinary between plasma chemistry and medicine, are considered. It was shown that complex biological processes in living tissues and bodies can be controlled, stimulated, catalyzed, and diagnosed with the use of low-temperature, atmospheric-pressure air plasma. It was found that discharge plasma can produce the desired therapeutic effect in wound sterilization and healing, as well as in treatment of some skin diseases. The action of plasma is harmless for the human body under definite conditions and exerts a targeted, nondestructive therapeutic effect.     

Free Radicals Resulting from Plasma Polymerization and Plasma Treatment

A glass tube is subjected to plasma treatment (non-polymerizable plasma) or plasma coating (polymerizable plasma). Unpaired spins generated in the glass substrate alone, and in both substrate and coating for the second case, are detected by ESR It is shown that for both polymerizable and nonpolymerizable plasmas the substrate's unpaired spins (glass radicals) are caused, in large part, by UV radiation from the plasma. In the case of plasma coating, the glass radicals are formed at the outset of the polymerization because the coating increasingly absorbs the UV radiation as deposition continues. High concentrations of free radicals in the coating appear to be correlated with a high tendency to polymerize, while high values of substrate radical surface concentration are related to high levels of UV intensity in the plasma.     

Plasma Grooving System Using Atmospheric Pressure Surface Discharge Plasma

To fabricate narrow front contact grooves on a single crystalline silicon solar cell, we carried out etching of a silicon nitride film on a silicon substrate using the surface discharge plasma operated at atmospheric pressure. The control of groove width by changing the discharge voltage (V _d) and the length of a back electrode (l) used for formation of the surface discharge was examined. It was found that narrower electrode grooves could be obtained when l was short. For the case of l = 2 mm, the narrowest groove of 116 μm was obtained at V _d = 3.5 kV and the processing time (t _e) of 10 s.     

The Roles of Various Plasma Active Species in Toluene Degradation by Non-thermal Plasma and Plasma Catalysis

Plasma Chemistry and Plasma Processing - Investigating the roles of plasma active species in plasma chemical reaction process can improve understanding of the mechanism of volatile organic...     

Plasma spraying of alumina: Plasma and particle flow fields

A comprehensive experimental examination of the interaction between a subsonic thermal plasma jet and injected alumine, particles is presented. Measurements of plasma velocity, temperature, and entrained air were obtained from an enthalpy probe and mass spectrometer combination. A diffusive separation, or demixing, of the Ar and He plasma gas was observed. Centerline plasma velocities and temperatures ranged from 1501500 m/s and 2000 to 14,000 K, respectively, in the region between the torch and a typical substrate location of 90 mm. Measurements of particle size, velocity, tempearture and local number density were obtained from a combination laser particle sizing system, Laser doppler velocimeter (LDV), and two-color pyrometer. Centerline temperatures and velocities for the nominally 30 m particles used were 2400–2800 K and 150–200 m/s, respectively.     

Cold Plasma Processing and Plasma Chemistry of Metallic Cobalt Surface

Plasma processing of metallic cobalt was experimentally investigated with three fluorine-containing gases, CF₄–O₂, SF₆–O₂, and NF₃ to determine the surface decontamination rate and to examine the reaction mechanism. Results show that the maximum etching rate reaches 17.12 μm/min with NF₃ gas at 420°C, while the rates are 2.56 μm/min and 1.14 μm/min with CF₄–O₂ and SF₆–O₂ gas, respectively, at the same temperature. AES analysis identified the constituent elements of the reaction products to be oxygen, fluorine, and cobalt, and XPS analysis reveals that the reaction product with all three plasma gases is very likely to be CoF₂.     

Transport Coefficients in Water Plasma: Part I: Equilibrium Plasma

Knowledge of the transport coefficients of steam water plasma is important for modeling plasma flow processes and heat transfer. In this study, calculations of these properties were performed in a temperature range from 400 to 30,000 K and at pressures of 0.5, 1.0, 5.0 and 10 bar. Herein the composition of water plasma was determined at equilibrium. First, the most recent data on potential interactions and elastic differential cross sections for interacting particles were carefully examined in order to choose those most appropriate for determining the collision integrals. Second, we restricted the number of species to ten (e, H, O, H⁺, O⁺, O⁺⁺, H₂, O₂, OH and H₂O) and tested our collision integrals by comparing the thermal conductivity and viscosity to experimental data for water (at low temperatures). Finally, the total thermal conductivity, viscosity and electrical conductivity were calculated for different pressures.