羊水中锌铜铁锰钙的测定

对61例妊娠晚期(孕34～40周)孕妇羊水进行了微量元素锌、铜、铁、锰及常量元素钙的测定.测定结果依次为:锌0.938±0.631 mg/L,铜0.178±0.156 mg/L,铁1.471±0.706 mg/L,锰0.047±0.017 mg/L,钙56.4±22.9 mg/L,为羊水微量元素研究提供了参考.     

Analyse Hydrometallurgique et Caracterisation de Miner Secondaires

Abstract

Two copper ores (containing between 1% and 2% of the metal) were analyzed by UV emission spectroscopy, infrared spectroscopy and X-ray diffraction yielding - per se - inconclusive results. The ores were subsequently classified by particle size into three “granular fractions”. Determination of copper, dissolved from each fraction by anaerobic and aerobic digestion with 5% aqueous sulphuric acid, produced illuminating information on the presence of sulfide-and oxide-type copper compounds. Fractionation was further refined by magnetic separations.     

Investigation of pituitary adenylate cyclase activating polypeptide in human gynecological and other biological fluids by using MALDI TOF mass spectrometry

Pituitary adenylate cyclase activating polypeptide (PACAP) is a multifunctional and pleiotropic neuropeptide. PACAP has diverse effects in the endocrine system, among others, it plays important roles in oogenesis, implantation and development of the nervous system. However, it is not known whether PACAP is present in the fluids of the human reproductive organs. The aim of the present study was to determine, by means of mass spectrometry and radioimmunoassay, whether PACAP is present in human amniotic fluid, ovarian follicular fluid and cervico-vaginal fluid. Samples were obtained from healthy adult volunteers. Our MALDI TOF and MALDI TOF/TOF spectrometry results show that PACAP38 is present in all of the follicular fluid samples, and PACAP-like immunoreactivity was also measured by radioimmunoassay. However, we did not find the characteristic peak representing the unmodified 38 amino acid form of the peptide in normal cervico-vaginal smear and amniotic fluid samples. Furthermore, we analyzed other body fluids for comparison, such as human nasal fluid, saliva and aqueous humor. PACAP was not found in these latter samples. In summary, the present study provides evidence for the presence of PACAP in human follicular fluid, suggesting a role in oocyte function, but determination of the exact physiological significance awaits further investigation.     

妊娠晚期羊水中微量元素测定及其与胎儿生长发育关系的研究

对１０２名足月正常妊娠第一胎的产妇妊娠晚期羊水中６种微量元素（锌、铜、锰、铁、钙、镁）首次进行了测定，并通过对出生新生儿生长发育的监测探讨其与胎儿生长发育的关系。妊娠晚期羊水中６种微量元素含量（±Ｓ／×１０－５）分别为：Ｚｎ２．２９±１．７７，Ｃｕ０．１４±０．１４，Ｍｎ０．１３±０．２３，Ｆｅ３．６９±２．７０，Ｃａ８２．５４±７４．１８，Ｍｇ１８．７１±１１．０９．男女新生儿其母羊水中微量元素含量比较无显著差异，Ｐ≥０．０５．与文献报道中期妊娠羊水中所含微量元素比较有增加趋势．６种微量元素相互关系中．与锌、钙呈正相关外，锌与铜、锰、铁、镁呈负相关．低体重组与低身长组新生儿孕母羊水中锌含量明显低于高体重组和高身长组，有显著差异，Ｐ≤０．０１．铁在高身长组含量增高，与低身长组比较有显著差异，Ｐ≤０．０５．锰于低体重组含量升高，与高体重组比较有显著差异，Ｐ≤０．０１．镁与铜于低身长组含量升高，与高身长组比较有显著差异，Ｐ分别≤０．０５与０．０１．可见高铜、高锰、高镁可致胎儿生长发育迟缓．     

Selectivity and efficiency enhancement of supercritical fluid extraction by application of reactive additives. I. The analysis of calcium montanate using citric acid as a complexing agent

It has been demonstrated that calcium montanate (a mixture of aliphatic hydrocarbons, fatty acid esters of C₂₈–C₃₂ acids, the calcium salts of these fatty acids, and the acids themselves) can be selectively extracted with supercritical fluids. By use of carbon dioxide, carbon dioxide containing 10% methanol, and carbon dioxide containing 10% methanol and citric acid (as a further additive), the various compound classes could be isolated with high selectivity. The addition of citric acid results in the complexation of Ca²⁺ and the simultaneous formation of the free fatty acids, which are soluble in the extractant.     

Investigation of low mass oligomers and polymer additives from plastics. Part II: Application to polyolefin soxhlet extracts

Polyolefin Soxhlet extracts have been investigated by capillary SFC using flame ionization detection. Separation and detection of every polymer additive (antioxidants, antistatic agents, etc.) present in the plastic were possible, sometimes in a single CSFC run. Identification of coextracted low mass oligomers and certain of the alteration products of Irganox 1010 was confirmed by GC-MS. New methods are presented for the determination of reacted and remaining calcium stearate, used in plastics both as a stabilizer and a lubricant.     

Direct and Rapid Electrochemical Determination of Total Surfactants in Amniotic Fluid for Assessment of Foetal Lung Maturity

Abstract

The characteristic response in the polarographic current-time curves, observed by the inhibition of the oxygen reduction process by adsorption of phospholipids at the mercury-solution interface, is used for the direct and rapid analysis of surfactants content in amniotic fluid samples. Good correlations were obtained between the described method and two well established routine methods used for estimation of foetal lung maturity in prenatal diagnosis of the respiratory distress syndrome.     

Supercritical fluid extraction / capillary supercritical fluid chromatography / Fourier transform infrared microspectrometry of polycyclic aromatic compounds in a coal tar pitch

The combination of supercritical fluid extraction, high resolution capillary supercritical fluid chromatography, and Fourier transform infrared microspectrometry is described for the separation and identification of polycyclic aromatic hydrocarbons in a coal tar pitch. The variable solvating power of the supercritical fluid was utilized to selectively fractionate the sample. The fluid extract was decompressed through a frit restrictor into the sample cavity of a cooled microvalve injector, where the analytes were deposited and concentrated for subsequent chromatographic analysis. Several of the analytes separated in the chromatograph were collected on a potassium bromide disc at a solvent elimination inter-face for subsequent infrared analysis involving the use of an infra-red microscope accessory. The spectra obtained show the power of this detection technique for distinguishing between isomers.     

Retention in capillary supercritical fluid chromatography

Supercritical fluid chromatography (SFC) sometimes exhibits GC-like behavior and sometimes LC-like behavior, depending on conditions. However, it is not always clear whether one of these types of behavior, or a combination, operates for a particular set of conditions for every solute in a mixture. For example, some components may be partitioned mostly by their vapor pressures, while others, in the same mixture, are partitioned predominantly by solvent-like properties of the mobile phase. Plots of retetion (as log of the capacity factor) vs. reciprocal temperature at constant pressure reveal a clear change in the character of the separation of well-behaved solutes. A thermodynamic explanation of the observed behavior is given, based on the assumption that partitioning is controlled by the heats of solution of solute in the mobile and stationary phases. A model of SFC retention as it deviates from pure-GC behavior on the same column is presented.     

About the physical validity of attaching the repulsive terms of analytical EOS models by temperature dependencies

This study demonstrates that any temperature dependency introduced in the term describing the inter-molecular repulsive forces of analytical EOS models leads to prediction of the infinite value for the isochoric heat capacity at the density limit conditions. The temperature-dependent hard sphere diameters and co-volumes necessarily result in the non-physical negative infinite values of this property at the infinite pressure, which in turn leads to the non-physical predictions of other properties, such as the sound velocities. In addition, this study demonstrates that the inconsistency existing at the imaginary state of infinite pressure may have a very strong negative impact on predicting the data of real fluids at the experimentally available pressures. Therefore making the repulsion compressibility factor temperature-dependent seems highly non-recommended.     

Comparison by capillary SFC and SFC-MS of soxhlet and supercritical fluid extraction of hamster feces

Components of hamster feces ranging from low molecular weight fatty acids through the expected range of triglycerides have been eluted in a single SFC run with simultaneous pressure and temperature programming. Temperature programming from 140°C to 240°C was required to provide optimum conditions for separation of the fatty acids and to move the elution region of the sterol esters away from that of the triglycerides. Data from chemical ionization and electron impact mass spectrometry of compounds separated by SFC were used to confirm identities suggested by retention measurements and to provide tentative identities of unknown compounds. SFC with flame ionization detection was used to compare Soxhlet extraction, off-line supercritical fluid extraction (SFE), and on-line SFE of the feces. Although samples obtained by Soxhlet extraction and SFE produced very similar chromatograms, SFE required far less time and consumed much smaller quantities of organic solvent.     

Supercritical fluid extraction of 2,3,7,8-tetrachlorodibenzo-p-dioxin from sediment samples

Supercritical fluid extraction (SFE) is a promising technique for the extraction of 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD) from environmental matrices such as contaminated sediments. The ability of SFE to solubilize many organic contaminants is well documented in industrial processes but its analytical applications were exploited just recently. In this study supercritical carbon dioxide and nitrous oxide and their mixtures with 2% methanol were used to extract 2,3,7,8-TCDD from aquatic sediments. An attractive feature of this process is that the carbon dioxide, being a virtually inert fluid, leaves no solvent residue on the processed sediment. Almost 100% of the 2,3,7,8-TCDD can be extracted from a sediment spiked with 200 μg/kg 2,3,7,8-TCDD in 30 minutes by using supercritical carbon dioxide + 2% methanol. Cleanup procedure is compared with the Soxhlet extraction procedure currently used as a standard method for extracting dioxins from sediment samples.     

Analysis of propellant stabilizer components via packed and capillary supercritical fluid chromatography/Fourier transform infrared spectrometry

The separation of model mixtures of nitrated diphenylamine and nitrated aniline via supercritical fluid chromatography employing both capillary and packed columns is described. With highly deactivated stationary phases each mixture could be separated with 100% CO₂ pressure programmed. Peak identification and peak purity were afforded by on-line Fourier transform infrared spectrometric detection. Nitrosoaniline derivatives were observed via FTIR to have been converted to nitro derivatives on storage.     

Synergy between adiponectin and interleukin-1β on the expression of interleukin-6, interleukin-8, and cyclooxygenase-2 in fibroblast-like synoviocytes

To determine whether adiponectin may have synergistic effects in combination with the proinflammatory cytokine interleukin (IL)-1β regarding the production of proinflammatory mediators during arthritic joint inflammation, synovial cells from rheumatoid arthritis (RA) patients were treated with adiponectin, IL-1β, and their combination for 24 h. Culture supernatant was collected and analyzed by enzyme-linked immunosorbent assay for levels of IL-6, IL-8, prostaglandin E(2) (PGE(2)), vascular endothelial growth factor (VEGF), and matrix metalloproteinases (MMPs). Adiponectin-mediated intracellular signaling pathways were investigated to elucidate the molecular mechanisms underlying their synergy. The association of proinflammatory mediators with adiponectin was investigated in the synovial fluid of arthritis patients. Adiponectin functioned synergistically with IL-1β to activate IL-6, IL-8, and PGE2 expression in RA fibroblast-like synoviocytes; Levels of VEGF, MMP-1, and MMP-13 were not synergistically stimulated. Adiponectin and IL-1β each increased the expression of both adiponectin receptor 1 and IL-1 receptor 1. However, adiponectin and IL-1β did not synergistically support the degradation of IκB-α or the nuclear translocation of NF-κB. Synergistically increased gene expression was significantly inhibited by MG132, an NF-κB inhibitor. Supporting the in vitro results, IL-6 and IL-8 levels were positively associated with adiponectin in synovial joint fluid from patients with RA, but not osteoarthritis (OA). In conclusion, adiponectin and IL-1β may synergistically stimulate the production of proinflammatory mediators through unknown signaling pathways during arthritic joint inflammation. Adiponectin may be more important to the pathogenesis of RA than previously thought.     

Addressing the issue of numerical pitfalls characteristic for SAFT EOS models

This study demonstrates the SAFT models can have doubtless advantages in predicting thermodynamic properties comparing to cubic equations of state. However they might be affected by two kinds of numerical pitfalls, namely the erroneous shapes of their isotherms resulting in the multiple phase equilibria predicted for pure compounds, and the undesired consequences of attaching their reduced densities by temperature dependencies. The latter are the negative heat capacities at very high pressures and the intersections of isotherms. Some versions, such as the SAFT of Chapman et al. [17] and SAFT-VR-SW of Gil-Villegas et al. [19] are found to be free of the pitfalls of the 1st kind. However the unsafe temperature dependencies are still essential for their accuracy. The present study proposes a modification of the Carnahan-Starling repulsive term maintaining the reduced densities temperature-dependent while making the covolumes temperature-independent. It is demonstrated that this manipulation might address the problem of numerical pitfalls and preserve the outstanding performance of the models.     

Glycolipid class profiling by packed-column subcritical fluid chromatography

The potential of packed-column subcritical fluid chromatography (SubFC) for the separation of lipid classes has been assessed in this study. Three polar stationary phases were checked: silica, diol, and poly(vinyl alcohol). Carbon dioxide (CO2) with methanol as modifier was used as mobile phase and detection performed by evaporative light scattering detection. The influence of methanol content, temperature, and pressure on the chromatographic behavior of sphingolipids and glycolipids were investigated. A complete separation of lipid classes from a crude wheat lipid extract was achieved using a modifier gradient from 10 to 40% methanol in carbon dioxide. Solute selectivity was improved using coupled silica and diol columns in series. Because the variation of eluotropic strength depending on the fluid density changes, a normalized separation factor product (NSP) was used to select the nature, the number and the order of the columns to reach the optimum glycolipid separation.