Direct coupling of capillary supercritical fluid chromatography with double-focusing high resolution mass spectrometry

An integral restrictor interface with jet separator for coupling capillary column supercritical fluid extraction – supercritical fluid chromatography with high resolution mass spectrometry (SFE-SFC-MS) has been built and used for the analysis of a fatty acid ester, and of polymer additives with a wide range of masses. The mobile phase used was supercritical carbon dioxide; a flame ionization detector (FID) was used in parallel with the mass spectrometer. Different SFC-MS interface operating conditions, e.g. temperature, restrictor position, flow rate, and sample transfer conditions were optimized to obtain good sensitivity and separation for these applications. In addition, the sensitivity of measurements performed with the direct insertion probe and by SFC-MS interface have been compared.     

毛细管气相色谱法测定油中植物甾醇和胆固醇

采用2.0mol/L的氢氧化钾乙醇溶液在85℃水浴上皂化45min，石油醚萃取，毛细管气相色谱法分离植物甾醇和胆固醇的分析方法，讨论并确定了样品皂化的最佳条件。用该法测定了芝麻油中甾醇的含量，相对标准偏差为0.86%-4.13%；回收率为89.59%-103.09%。结果表明：采用该方法具有操作快速、简便、准确等优点。     

固相微萃取技术与环境样品前处理

固相微萃取技术是80 年代末发展起来的一项新型的无溶剂化环境样品前处理技术, 它主要与气相色谱和高效液相色谱联用, 能快速和有效地分析环境样品中的痕量有机污染物。技术从出现至今主要在萃取装置(萃取纤维涂层)、萃取方式及后序分析仪器上有较大的发展和变化, 这使得技术的应用范围不断拓宽。通过对现有文献的总结, 本文还提出了固相微萃取技术今后的发展趋势。     

Isolation of new quinidine metabolites and simultaneous determination of quinidine and its metabolites in blood and urine by direct injection HPLC analysis

Summary New quinidine metabolites, including 10,11-dihydrodiol quinidine N-oxide, 10,11-dihydrodiol quinidine and their glucuronides, were found in human urine. A quinidine monitoring HPLC method including these metabolites, is proposed by the direct injection of body fluid samples onto the precolumn for deproteinization followed by reverse phase separation in the analytical column with a column switching technique. The recovery of spiked quinidine and its metabolites in plasma was quantitative (98–102%) with good reproducibility (C.V.: 1.6–4.0%). Several clinical samples such as whole blood and urine were analyzed by the present method.     

反相高效液相色谱-蒸发光散射检测法测定紫苏子油中的α-亚麻酸

建立了反相高效液相色谱-蒸发光散射检测器(RP-HPLC-ELSD)测定紫苏子油中α-亚麻酸含量的方法。紫苏子油样用0.5 mol/L的KOH-CH3OH溶液于60 ℃水浴中皂化20 min、6 mol/L的盐酸酸化后用无水乙醚萃取,再用氮气流吹干乙醚，用甲醇溶解并定容,然后直接进行RP-HPLC-ELSD分析。结果表明,当α-亚麻酸质量为6.2～45.4 μg时,其峰面积A的对数(lg A)与α-亚麻酸质量m(μg)的对数(lg m)呈线性关系,线性方程为lg A=1.3675·lg m－1.628,相关系数为0.9973(n＝5)。以信噪比S/N=3计算,方法的检出限为0.11 μg。被分析的紫苏子油中α-亚麻酸的含量为6.79%(质量分数),相对标准偏差(RSD)为5.1%(n=5)；平均回收率为102%,RSD为6.3%(n=5)。该方法简单、快速、准确。     

高温凝胶渗透色谱仪中气泡的排除

叙述了高温凝胶(渗透)色谱(GPC)的流动相中出现气泡时的现象,指出气泡的出现对仪器运行和样品测试的影响,以及排除气泡的方法和过程.对可能出现气泡的原因进行了分析,讨论了避免出现气泡现象需要注意的问题和采取的措施.     

亲和层析在蛋白质研究中的应用进展

文中介绍了生物、免疫、固定化金属离子拟生物几类常规亲和层析的原理及其在蛋白质分离纯化以及分析鉴定方面的应用（引用文献25篇）。