伯胺N1923萃取色谱法分离硫酸介质中钪,铁,钛的研究

本文研究了Ｎ１９２３为固定相分离硫酸介质中钪、铁、钛的萃取色谱体系，流动相采用２ＭＨ２ＳＯ４－２ＭＨ２ＳＯ４＋Ｈ２Ｏ２－２ＭＨＣｌ三段淋洗能将三元素完全分离；又研究了Ｎ１９２３－ＴＢＰ二元固定相的分离情况，采用２ＭＨ２ＳＯ４＋Ｈ２Ｏ２－２ＭＨＣｌ二段淋洗，铁钛被同时淋出后与钪完全分离。钪回收率分别为１０７％和９８％。     

高效液相色谱法和因子分析—紫外光度法测定荧光增白剂中两种成分

本文采用两种同时测定荧光增白剂工业产品中，１，４－（２，４′－氰基苯乙烯基）苯（记为ＥＢ）和异构体１，４－双（２－氰基苯乙烯基）苯（记为ＥＲ）两组分的方法，一种是ＨＰＬＣ法，采用Ｓｈｉｍ－ｐａｃｋＣＬＣ－ＳＩＬ柱（５μｍ，６．０ｍｍｉ．ｄ×１５０ｍｍ）正己烷－乙酸乙酯（９０：１０Ｖ／Ｖ）为流动相，流速２ｍＬ／ｍｉｎ，柱温３０℃检测波长ＵＶ３６０ｎｍ方法简单，准确，快速，另一种是因子分析－紫外光度法     

在不同体积比流动相及不同缓冲溶液中毛细电色谱ODS柱的分离行为

１引言毛细电色谱中，流动相的选择同样取决于固定相及被分离样品。对于ＯＤＳ柱，若分离中性样品时，通常选择一定体积比的有机相和无机缓冲溶液混合，如一定百分比的ＣＨ３ＣＮ和一定百分比的Ｎａ２Ｂ４Ｏ７水溶液。流动相浓度配比不同时，样品在固定相上的保留不同，进而造成分离时间和选择性不同。笔者通过实验观察到，当在同样浓度的有机相中加入的缓冲溶液不同时，固定相对样品的分离能力也不尽相同。本文即以实验为依据，分别讨论ＯＤＳ柱在不同体积比流动相及在相同体积比流动相，不同缓冲溶液下的分离行为。２实验部分２．１仪器与…     

2,2,2-三氟-1-(9-蒽基)乙醇对映体在涂敷型手性固定相上的拆分

用高效液相色谱法在涂敷１５％（Ｗｔ）三苯基氨基甲酸纤维素醌手性柱上,考察了洗脱液正己烷／醇（Ｖ／Ｖ）中醇对分离－２,２,２－三氟－１（９－蒽基）乙醇对映体的影响,初步认为,在对映体分离过程中,洗脱液中醇与手性固定相的ＮＨ和Ｃ＝Ｏ形成氢键作用,此过程与对映体和手性固定相的ＮＨ和Ｃ＝Ｏ所形成氢键作用相竞争;洗脱液中醇的结构不同之所以影响对映体的分离效果,还与洗脱中醇改变固定相中手性空穴的立体环境有关,     

伯胺N1923苹取色谱法分离硫酸介质中钪、铁、钛的研究

本文研究了Ｎ１９２３为固定相分离硫酸介质中钪、铁、钛的萃取色谱体系，流动相采用２ＭＨ２ＳＯ４－２ＭＨ２ＳＯ４＋Ｈ２Ｏ２－２ＭＨＣｌ三段淋洗能将三元素完全分离；又研究了Ｎ１９２－ＴＢＰ二元固定相的分离情况，采用２ＭＨ２ＳＯ４＋Ｈ２Ｏ２－２ＭＨＣｌ二段淋洗，铁钛被同时淋出后与钪完全分离。钪回收率分别为１０７％和９８％。     

红豆杉提取液中紫杉醇的HPLC法测定

建立了高效液相色谱法（ＨＰＬＣ）测定云南红豆杉原始提取液中紫杉醇含量的方法，经比较Ｃ１８和氰基固定相，发现在氰基柱上，以ＭｅＯＨ－ＭｅＣＮ－Ｈ２Ｏ（２０：１６：６４体积分数）为流动相时，紫杉醇获得更满意的分离、流速２．０ｍＬ／ｍｉｎ，柱温４０℃，ＵＶ检测波长：２２７ｎｍ，方法简便、准确、适合于微量紫杉醇的测定。     

气相色谱法的限制因素

本文根据气相色谱柱前，柱后蒸汽压的变化，通过对含不同碳原子的６类化合物于不同温度下蒸汽压的研究，提出采用气相色谱法时组分的蒸汽压必须高于１５－７４６Ｐａ，容量因子ｋ＾１必须在０．２－２０之间。运用相应碳链长度（ＣＣＣＬ）的概念，通过固定相特性参数（Ｖｇ（７）和Ａ１）解决了一定温度下“什么组分可从气相色谱柱中流出？“的预测问题。结合检测器特性得出是保留值太大限制了组分采用气相色谱法，阐明了只要组分能     

高效液相色谱法测定荧光增白剂OB

本文建立了高效液相色谱测定荧光增白剂ＯＢ，即２．５－双（５－叔丁基－２－苯并恶唑基）噻吩的方法。采用ＹＷＧ Ｃ１８色谱柱，四氢呋喃－水（６７：３３Ｖ／Ｖ）为流动相，流速１．０ｍＬ／ｍｉｎ，紫外检测波长３６０ｎｍ，柱温４０℃，分离时间少于１１ｍｉｎ。应用于工业产品的测定，结果满意。     

一种非晶硅膜改性弹性玻璃毛细管交联中等极性固定相色谱柱的制备

研究了非晶硅膜改性的弹性玻璃毛细管交联ＯＶ－１７０１中等极性固定相色谱柱。在适当温度下，采用过氧化二异丙苯（ＤＣＵＰ）游离基引发交联ＯＶ－１７０１固定液，成功地制备了交联ＯＶ－１７０１柱，该柱具有柱效高、惰性好、耐溶剂、抗腐蚀和耐高温等性能，是一种新型高性能的中等极性交联柱。     

固定化有机改进剂RP－HPLC固定相的研究

通过在ＲＰＨＰＬＣ固定相Ｃ１８表面键合氨基硅烷，引入氨基基团，将有机改进剂固定至硅胶键合相表面，克服了固定相表面硅羟基对含氮有机化合物的不可逆吸附。以最简单的ＣＨ３ＯＨ－Ｈ２Ｏ洗脱体系即能获得含氮有机和的最佳分离，从而可简化分离操作，提高柱寿命，降低分离成本。     

单萜/顺丁烯二酸酐加成物及其酯类衍生物的气相色谱法分析

 摘要：研究了单萜/顺酐加成物及其酯化衍生物在OV-17和SE-30柱上的某些色谱性能和定量分析的线性相应关系。结果表明,这两种化合物在涂渍量为5％～10％的OV-17和SE-30柱上均能正常出峰;在峰形对称性和出峰时间上,OV-17柱具有优势。260℃以后,色谱峰面积与汽化温度无关。     

Palladium(II) chelate of tetradentate Schiff base as mixed stationary phase for gas chromatography

Bis(acetylacetone)ethylenediiminepalladium(II) (PdAA2en) was examined as a mixed stationary phase with OV-1 on Chromosorb G/NAW 60-80 mesh size for the GC separation of aromatic hydrocarbons, heteroaromatics, alcohols, aldehydes, ketones, esters, and nitro compounds. Forty-two compounds were examined and the GC results were compared with those obtained with 3% OV-1 on Chromosorb G/NAW 60-80 mesh size under similar operating conditions. Improved resolution, peak asymmetry, theoretical plate numbers, and Kovats indices were obtained on the mixed stationary phase of 3% OV-1 + 5% PdAA2en compared to 3% OV-1 column. The stability constant (Km), enthalpies (deltaH), entropies (deltaS), and Gibbs free energies (deltaG) of the GC elution on the column (2 m x 3 mm id) packed with 3% OV-1 + 5% PdAA2en on Chromosorb G/NAW 60-80 mesh size have been calculated. Donor-acceptor complexation in the gas phase is indicated by negative values of enthalpy (-deltaH) within 5.81 to 10.89 kcal/mol and Gibbs free energy (-deltaG) from 1.34 to 4.08 kcal/mol. The retention time transformations on both the phases were calculated and the ratios obtained from the stationary phases 3% OV-1 and 3% OV-1 + 5% PdAA2en were plotted on the x-axis and the y-axis, respectively, and the coefficients of determination for alkanes, aromatic and heteroaromatics, ketones, and alcohols were observed to lie within 0.5253 to 0.9742, indicative of some different kinds of interaction of the two stationary phases with the solutes.     

涂渍极性及强极性固定相硅膜改性弹性玻璃毛细管柱的研制

本文工作研究了极性、强极性固定液直接涂渍在硅膜改性弹性玻璃毛细管内壁上，经优化温度老化色谱柱，成功地研制出ＯＶ－２２５，ＤＥＧＳ，Ｓｉｌａｒ５，Ｓｉｌａｒ９，Ｓｉｌａｒ１０等硅膜改性弹性玻璃毛细管柱，各种柱子均具有柱效高，热稳定性好的色谱性能。     

Effect of extra-column volume on practical chromatographic parameters of sub-2-μm particle-packed columns in ultra-high pressure liquid chromatography

Effects of extra-column volume on apparent separation parameters were studied in ultra-high pressure liquid chromatography with columns and inlet connection tubings of various internal diameters (id) using 50-mm long columns packed with 1.8-μm particles under isocratic conditions. The results showed that apparent retention factors were on average 5, 11, 18, and 41% lower than those corrected with extra-column volumes for 4.6-, 3.0-, 2.1-, and 1.0-mm id columns, respectively, when the extra-column volume (11.3 μL) was kept constant. Also, apparent pressures were 31, 16, 12, and 10% higher than those corrected with pressures from extra-column volumes for 4.6-, 3.0-, 2.1-, and 1.0-mm id columns at the respective optimum flow rate for a typical ultra-high pressure liquid chromatography system. The loss in apparent efficiency increased dramatically from 4.6- to 3.0- to 2.1- to 1.0-mm id columns, less significantly as retention factors increased. The column efficiency was significantly improved as the inlet tubing id was decreased for a given column. The results suggest that maximum ratio of extra-column volume to column void volume should be approximately 1:10 for column porosity more than 0.6 and a retention factor more than 5, where 80% or higher of theoretically predicted efficiency could be achieved.     

Alltech集束毛细管柱和常规毛细管柱的比较

对集束毛细管气相色谱柱的色谱性能,如流速对柱效的影响、柱温对柱效的影响、柱容量等进行了考察,并将其对典型火炸药成分ＤＮＴ,ＴＮＴ的分离与常规毛细管气相色谱柱进行了比较。结果表明,集束毛细管气相色谱柱综合了填充柱与石英毛细管气相色谱柱之优点,弥补了二者的不足,是一种柱容量较大且分离效能好、可以在高载气流速下操作的新型气相色谱柱。     

Supercritical fluid chromatography of metoprolol and analogues on aminopropyl and ethylpyridine silica without any additives

Metoprolol and a number of related amino alcohols and similar analytes have been chromatographed on aminopropyl (APS) and ethylpyridine (EPS) silica columns. The mobile phase was carbon dioxide with methanol as modifier and no amine additive was present. Optimal isocratic conditions for the selectivity were evaluated based on experiments using design of experiments. A central composite circumscribed model for each column was used. Factors were column temperature, back-pressure and % (v/v) of modifier. The responses were retention and selectivity versus metoprolol. The % of modifier mainly controlled the retention on both columns but pressure and temperature could also be important for optimizing the selectivity between the amino alcohols. The compounds could be divided into four and five groups on both columns, with respect to the selectivity. Furthermore, on the aminopropyl silica the analytes were more spread out whereas on the ethylpyridine silica, due to its aromaticity, retention and selectivity were closer. For optimal conditions the column temperature and back-pressure should be high and the modifier concentration low. A comparison of the selectivity using optimized conditions show a few switches of retention order between the two columns. On aminopropyl silica an aldehyde failed to be eluted owing to Schiff-base formation. Peak symmetry and column efficiency were briefly studied for some structurally close analogues. This revealed some activity from the columns that affected analytes that had less protected amino groups, a methyl group instead of isopropyl. The tailing was more marked with the ethylpyridine column even with the more bulky alkyl substituents. Plate number N was a better measure than the asymmetry factor since some analyte peaks broadened without serious deterioration of symmetry compared to homologues.     

Preparation and evaluation of OV-240-OH coated glass capillary columns for isomer specific determination of PCDDs and PCDFs

Glass capillaries were leached, dehydrated, persilylated with 1, 3-bis (3-cyanopropyl) tetramethyldisiloxane, and coated with OV-240-OH. After crosslinking and binding the phase to the glass surface the columns showed high separation efficiency, high temperature stability, and inertness comparable to persilylated apolar columns. Column performance is shown to be superior to liquid phase cyanopropyl columns such as SP 2330. The excellent separation capabilities together with the selectivity of the phase makes OV-240-OH coated columns a valuable tool for the determination of toxic isomers in complex mixtures of polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs). The order of elution of individual TCDD isomers was found to be similar to that described for SP 2330 or Silar 10c. The detection of PCDDs and PCDFs in a fly ash extract further illustrates the utility of OV-240-OH coated columns. The high temperature limit of these columns opens the way for the analysis of high boiling compounds such as mixed brominated/chlorinated dibenzo-p-dioxins and dibenzofurans.     

手性有序无机介孔硅用作气相色谱固定相

手性介孔材料在手性分离、不对称催化、手性传感等领域具有广泛的应用价值。手性有序无机介孔硅是一类介孔结构高度有序、不含有机成分的手性材料。该文采用D-苯丙氨酸为手性源合成手性有序无机介孔硅(COIMS),将其用聚硅氧烷(OV-1701)稀释后用作固定相制备毛细管气相色谱手性柱,并对该手性柱的分离性能进行了考察,8种手性化合物在该手性柱上得到了拆分。COIMS柱对直链烷烃、醇的分离也表现出良好的选择性。该柱还具有分析时间短、在较高温度下测定稳定等优点,其具有开发成高温手性固定相的潜力。     

Capillary gas chromatography of some metal acetylacetonates

Summary The retention and resolution of simple mixture of Al(III), Cr(III), Co(III), and Fe(III) acetylacetonates were investigated on capillary columns coated with methyl and methyl phenyl silicones (OV-1 or OV-17) used as the stationary phase, at different column temperatures and carrier gas flow rates. Successful elution and good resolution were obtained only for the Al(III) and Cr(III) complexes, both under isothermal and programmed-temperature conditions; better resolution was observed on the column coated with OV 17.     

丙烯腈中微量杂质的毛细管色谱法分析

提出了一种分析丙烯腈中微量杂质的大孔径ＯＶ－１０１和ＯＶ－１７ＳＣＯＴ串联柱及毛细管进样系统。结果表明串联柱具有寿命长和分离效率高的特点,定量分析误差小于４％。