Determination of low levels of an antioxidant in polyolefins by large-volume injection temperature-programmed packed capillary liquid chromatography

Sub-ambient column temperatures, promoting strong interactions between the analyte and the stationary phase material, were utilized to focus large volumes of the polyolefin antioxidant Irganox 1076 [benzenepropanoic acid, 3.5-bis(1,1-dimethylethyl)-4-hydroxy-, octadecyl ester] on the column inlet, using pure acetonitrile as sample solvent and mobile phase. Injection volumes up to 100 microl were successfully employed on a 50 cm x 320 microm I.D. capillary column packed with 5 microm Kromasil 100 ODS particles. Irganox 1076 was eluted after completed injection by temperature programming, using a temperature program from 7 to 90 degrees C, in 3 degrees C min(-1). UV detection, using a low-dispersion "U"-shaped flowcell, was performed at 280 nm. The method was applied for the determination of Irganox 1076 that was extracted from low-density polyethylene (0.6 ppm, w/w). Both Soxhlet and microwave-aided solvent extractions were performed, using chloroform and acetonitrile as solvents, respectively. The microwave-aided extraction with acetonitrile was found to give approximately the same yield as the standard Soxhlet reference method. Consequently, small volumes of acetonitrile could be used both as extraction solvent, sample solvent and mobile phase, simplifying the analysis process. The mass limit of detection of the method was found to be 3.3 ng, corresponding to a concentration limit of detection of 33 ng ml(-1), utilizing an injection volume of 100 microl. The within and between day precision of retention times displayed relative standard deviations below 1.2%.     

Stability of workroom air volatile organic compounds on solid adsorbents for thermal desorption gas chromatography

The storage stability of the occupationally frequently occurring compounds, methylethylketone, methylisobutylketone, benzene, toluene, tetrachloroethylene, n-butylacetate, -pinene, β-pinene, limonene and n-decane, has been investigated on the adsorbents Tenax TA, Chromosorb 106 and Carbotrap using thermally desorbable tube type samplers, commonly utilized in ambient and workroom atmospheric measurements. Fifty and 500 ng of each compound were loaded on the various adsorbents tubes, stored at both ambient (20 °C) and refrigerated (4 °C) temperatures and analysed by means of thermal gas chromatography with mass spectrometric detection on days 0, 7, 14 and 28 after exposure. A 90% storage recovery was chosen as acceptance criteria for storage stability, and statistical testing by Student's t-test, analysis of variance and Bonferroni post hoc tests were employed to investigate the effect of the categorical variables storage time, storage temperature and analyte loading on the different adsorbents. Chromosorb 106 showed the overall best behaviour with recoveries of 90% or better for all analytes during the 28-day test period. Tenax TA and Carbotrap yielded lower recoveries and were more influenced by variations in storage time, storage temperature and analyte loading. Refrigerated temperatures were best avoided for storage on Tenax TA, but may increase the recovery of some compounds on Carbotrap (e.g. n-butylacetate). The blank build-up on the adsorbents was also investigated, and Carbotrap and Tenax TA showed no signs of artefact development over time. Chromosorb 106, however, contained inherently more artefacts that build up over time, which in spite of the excellent storage capability, may limit its use in field studies where long storage times are normal.     

种植沙生植物--沙棘改善内蒙古地区生态环境

结合内蒙古地区现状，对沙棘的生物学和生态学特性、沙棘属植物化学成分和微量元素及种植沙生植物——沙棘的重要性和必要性进行了详细的研究和探讨。研究表明，沙棘属植物具有极强的生态适应性并富含多种营养成分和生物活性物质，并以耐干旱、耐瘠薄、萌蘖及固氮能力强等特点被称为治理非宜林地水土流失、改善生态环境的先锋树种。种植沙棘是治理内蒙古脆弱生态环境最经济、最有效的措施，是贫瘠的不毛之地发展经济、增加收入的经济树种。另外．种植沙棘的技术简便，容易掌握，投资少，见效快。     

Toward a general route to the eunicellin diterpenes: the asymmetric total synthesis of deacetoxyalcyonin acetate

A novel approach to the hydroisobenzofuran core utilizing a TiCl4-mediated [4+3] annulation is reported. This [4+3] annulation protocol provides a short, general route to the hydroisobenzofuran core present in the eunicellin diterpenes. Using this annulation, a short synthesis (17 steps) of deacetoxyalcyonin acetate, a member of the eunicellin family, has been achieved.     

内蒙古地区天然植物沙棘果中黄色素的提取工艺及性质研究

以内蒙古地区沙棘果实为原料，研究了提取黄色素的工艺条件，同时对该色素的性质进行了初步探讨。结果表明，以95％的乙醇溶液作浸提剂，提取的黄色素浓度最高，工艺流程简单易行，且无毒，无污染。对提取的黄色素进行的性质试验表明，沙棘黄色素对光、热具有较好的稳定性，适用于酸性或弱碱性的食品中，葡萄糖、氧化剂(H2O2)、还原剂(Na2SO3)等食品添加剂均无明显影响以上结果为这种优良天然色素的开发与应用提供了参考。     

A diastereoselective intramolecular hydroamination approach to the syntheses of (+)-, (+/-)-, and (-)-pinidinol

A diastereoselective, lanthanocene-catalyzed, intramolecular hydroamination reaction was applied to the preparation of 2,6-disubstituted piperidines. Various metal/ligand arrays in the catalysts were examined using a model substrate to allow optimization of the diastereoselectivity. It was determined that the relationship between metal size and ligand bulk plays an integral role in the transformation. The complex Cp2NdCH(TMS)2 converted 2-substituted 8-nonen-4-amines to 2,6-disubsituted piperidines with greater than 100:1 selectivity for the formation of the cis isomer. A short synthesis of pinidinol, an alkaloid isolated from various pine and spruce species, was then carried out to exploit this stereoselective reaction.     

Solid-Phase Synthesis of a Monofunctional trans-a(2)Pt(II) Complex Tethered to a Single-Stranded Oligonucleotide

Cross-linking ability is possible with the oligonucleotide-tethered, monofunctional trans-Pt(II) complex shown. It was synthesized by a novel solid-phase approach comprising conjugation of immobilized tetrathymidylic acid with a trans-a(2)Pt(II) building unit, ammonolysis, and transformation of the resulting complex (R=1-N-cyclohexylmethylthyminate) into the chloro derivative (R=Cl). a=NH(2)CH(3), T=thymine.