Rapid analysis of polymer homologues and additives with SFE/SFC-MS coupling

A rapid and easy analysis method for polymers is presented. The method involves sample preparation by SFE, separation of the extracted compounds by SFC and simultaneous quantitative detection by FID, as well as identification of unknowns by MS. The applications illustrate how structural research work and routine polymer analysis can be done with this time saving method.     

Volatile constituents of palm wine and palm sap

Palm wine and pasteurised palm sap volatiles were collected, concentrated on a Tenax GC and analysed by gas chromatography and gas chromatography-mass spectrometry. Eighty-two components were identified: 47 esters, 9 alcohols, 5 acids, 6 carbonyls, 2 acetals, 4 terpenes and 9 hydrocarbons. These had all been found previously in conventional wines. Odour evaluation of the separated palm wine components as they eluted suggested that no one compound is responsible for the characteristic palm wine odour. The acetates of higher alcohols and the ethyl esters of straight-chain aliphatic C₆-C₁₀ acids seemed to be important and may play a big role in imparting the fruity nuances of characteristic palm wine odour. Their association with alcohols seemed also to be necessary for the expression of typical palm wine odour. The qualitative difference between palm sap aroma and palm wine aroma appeared to be due mainly to the presence of these esters and alcohols in palm wine and their apparent absence from palm sap, as well as to the presence of some low-boiling esters and alcohols in palm sap and their apparent absence from palm wine.     

丙酰芸苔素内酯的气相色谱分析

采用毛细管柱气相色谱法,以(22E,24S) 2,22 二烯 5α 豆甾 6 酮为内标,对丙酰芸苔素内酯进行定量分析。色谱条件为12m× 0.53mm,膜厚1.5μm(CBP 1固定液)熔融石英毛细管柱,柱温为305℃,检测器、汽化室温度为320℃,载气流速为20mL/min。该方法检测丙酰芸苔素内酯质量分数的平均标准偏差为0.39%,平均回收率为100.4%。方法操作简便,定量准确。     

Contribution oftrans-18∶1 acids from dairy fat to european diets

Twelve commercial samples of French butter, purchased in October–November, and 12 other samples, purchased in May–June, were analyzed with particular attention to theirtrans-octadecenoic acid contents. The isomeric fatty acids were quantitated by a combination of gas-liquid chromatography (GLC) of total fatty acids as isopropyl esters on a polar capillary column (CPSil 88) and of silver nitrate-impregnated thin-layer chromatography followed by GLC of the pooled saturated (used as internal standards) andtrans-octadecenoic acid fractions. Autumn butters contained 3.22±0.44%trans-octadecenoic acids (relative to total fatty acids), whereas those collected during the spring contained 4.28±0.47% (P<0.01). Minimum and maximum values for the two sets of butters were 2.46 (autumn) and 5.10% (spring), respectively. The annual mean value for thetrans-octadecenoic acid content in all butter samples was 3.8% of total fatty acids (ca. 2% for thetrans-11 18∶1 acid). This value allows calculation of the daily individual intake oftrans-octadecenoic acids from dairy products by populations of member states of the European Economic Community (EEC). It varies from 0.57 g (Portugal) to 1.66 g (Denmark). The mean value for the twelve countries of the EEC is 1.16 g/person/d, which is close to data published for the United States. In France, the consumption oftrans octadecenoic acids from dairy fat is higher than that from margarines (ca. 1.5 vs. 1.1 g/person/d).     

工业层析洗梯液回收套用的一种方法

以生产甲胺基阿维菌素苯甲酸盐精品的工艺——工业层析产生的洗梯液回收套用的过程为例，说明利用二元恒沸物的组成随压力的变化而变化的规律，对生产洗梯液进行有效、简洁、合理分离及套用的方法。     

松辽盆地北部西斜坡区稠油成因与油源关系

松辽盆地北部西斜坡区分布的稠油资源是油气勘探的潜在领域。油藏流体地球化学分析表明，该地区稠油形成主要与厌氧细菌的生物降解作用有关。稠油的高温气相色谱分析，可以把稠油划分为2种成因类型、5个亚类。生物降解成因类型包括严重降解稠油、中等降解稠油和轻度降解稠油3个亚类；混合成因类型包括降解原油与原油蒸馏轻烃混合形成的稠油和降解原油与未降解原油混合形成的稠油2个亚类。生物标志化合物参数揭示的油岩关系表明，稠油来自斜坡东部的齐家—古龙凹陷的成熟烃源岩和该地区的未熟—低熟烃源岩，优越的油源条件为该地区稠油勘探展示了广阔前景。     

双氧水冷漂助剂液中润湿剂的分离和鉴测

双氧水冷漂助剂液中的润滑剂——烷基硫酸钠可以在四级氧化铝柱上用氯仿和乙醇—水的淋洗体系进行分离而获得纯品;用NMR和GC法进行结构分析;两相滴定法测定其含量。     

凝胶过滤色谱测定高分子量聚乙烯醇分子量和分子量分布

用凝胶过滤色谱对高分子量聚乙烯醇分子量、分子量分布进行剖析。采用Plaquagel-OH色谱柱,0.25mol/LNaNO3,0.01mol/L Na2HPO4-NaH2PO,pH=7的缓冲溶液流动相,流速1ml/min,示差折光检测器,柱温30℃,聚环氧乙烷作标准物。该方法能显著缩短分析时间,提高准确性,可用于对高聚合度聚乙烯醇进行研究和指导生产。     

Simultaneous HPLC quantification of total cholesterol,tocopherols and β-carotene in Barrosã-PDO veal

A simple, rapid and sensitive procedure for the simultaneous determination of total cholesterol, tocopherols and β-carotene in meat is described. The method involves a direct saponification of the meat, a single n-hexane extraction and the analysis of the extracted compounds by normal-phase HPLC, using fluorescence (tocopherols) and UV–Vis photodiode array (cholesterol and β-carotene) detections in tandem. Rates of recovery of spiked meat samples were 93% for cholesterol, 83–86% for (α-, β- and -γ) tocopherols and 89% for β-carotene. Repeatabilities were high (CV < 6%) for all determined compounds, except for δ-tocopherol. This tocopherol, which is not usually present in meat, showed a much lower recovery percentage (73%) and repeatability (12.8%). This methodology was applied for the quantification of total cholesterol, tocopherols and β-carotene in three muscles (longissimus thoracis, longissimus lumborum and semitendinosus) of the Portuguese traditional Barrosã-PDO veal, obtained from autochthonous calves fed extensively during summer (with the least abundant green pastures) and slaughtered in early autumn (October). Barrosã-PDO veal showed median contents of total cholesterol (0.50–0.56 mg/g) and, depending on the analysed muscle, moderate to high contents of α-tocopherol (3.3–3.9 μg/g) and β-carotene (0.07–0.09 μg/g), suggesting an high sensorial and hygienic quality.     

Preparation and adsorption behavior of a cellulose‐based,mixed‐mode adsorbent with a benzylamine ligand for expanded bed applications

A novel mixed‐mode expanded bed adsorbent with anion‐exchange properties was explored with benzylamine as the functional ligand. The cellulose composite matrix, densified with stainless steel powder, was prepared with the method of water‐in‐oil suspension thermal regeneration. High activation levels of the cellulose matrix were obtained with allyl bromide because of the relative inertness of the allyl group under the conditions of the activation reaction. After the formation of the bromohydrin with N‐bromosuccinimide and coupling with benzylamine, the activated matrix was derived to function as a mixed‐mode adsorbent containing both hydrophobic and ionic groups. The protein adsorption capacity was investigated with bovine serum albumin as a model protein. The results indicated that the prepared adsorbent could bind bovine serum albumin with a high adsorption capacity, and it showed salt tolerance. Effective desorption was achieved by a pH adjustment across the isoelectric point of the protein. The interactions between the cell and adsorbent were studied, and the bioadhesion was shielded by the adjustment of the salt concentration above 0.1M. Stable fluidization in the expanded bed was obtained even in a 2% (dry weight) yeast suspension. The direct capture of target proteins from a biomass‐containing feedstock without extra dilution steps could be expected with the mixed‐mode adsorbent prepared in this work, and this would be especially appropriate for expanded bed adsorption applications. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008