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991.
Determination of carbonyl compounds in air by HPLC using on-line analyzed microcartridges,fluorescence and chemiluminescence detection 总被引:1,自引:0,他引:1
Summary Sensitive and selective detection of dansylhydrazones of atmospheric carbonyl compounds (aldehydes and ketones) can be achieved using high performance liquid chromatography (HPLC) with fluorescence or chemiluminescence detection. The carbonyl compounds are derivatized by drawing air through small glass cartridges packed with porous glass particles impregnated with dansylhydrazine. After sampling, the contents of the cartridges are analyzed on-line by using a small plug of water (200 L) to transfer and focus the hydrazone derivatives at the head of a HPLC column. Greatly increased sensitivity over traditional methods derives from 1) analysis of the entire contents of the sampling cartridge, and 2) detection by fluoresence or peroxyoxalate chemilum-inescence. Results are compared for photo-initiated and H2O2-initiated peroxyoxalate chemiluminescence. This novel and practical system enables the detection of sub-ppbv concentrations of formaldehyde, acetaldehyde, acetone and higher carbonyls in air using relatively short sampling times. 相似文献
992.
Determination of estrogenic steroids in surface water and wastewater by liquid chromatography-electrospray tandem mass spectrometry 总被引:1,自引:0,他引:1
An analytical method is presented which permits trace level determination of 17alpha-ethynylestradiol (EE2), 17beta-estradiol (E2), and estrone (E1). Using this method, the estrogenic steroids were analyzed in drinking water, surface water, and wastewater (sewage influents and effluents) at concentrations down to 0.1 ng/L. Sample volumes between 100 and 500 mL are concentrated using automated solid-phase extraction. Analysis is performed by liquid chromatography with detection by tandem mass spectrometry. Applying simple clean-up procedures and internal standard calibration, recovery losses resulting from matrix-dependent ion suppression during electrospray ionization could be compensated for all of the investigated compounds. Recoveries around 100% were obtained for all analytes after correction using the internal standards. Limits of quantification (LOQ) were between 0.1 and 0.4 ng/L for purified sewage, surface, ground, and drinking water and between 1 and 2 ng/L in the case of raw sewage. Water treatment by wastewater treatment plants (WWTPs) or by a surface water treatment plant affected the removal of all estrogenic steroids. Thus, E1, E2, and EE2 were removed in the municipal WWTPs to the extent of 93%, 93%, and 80%, respectively. In the effluents of the WWTP in Ruhleben (Berlin, Germany), E1, E2, and EE2 were detected at the low ng/L level. E2 and EE2 were, however, not present in the Berlin surface water above the LOQ (0.2 ng/L). E1 was the only compound that could be detected in surface water samples. After additional surface water treatment it was still detectable but only at trace-level concentrations with a mean value of 0.16 ng/L. 相似文献
993.
Several varieties of blue ballpoint pen inks were analyzed by high performance liquid chromatography (HPLC) and infrared spectroscopy (IR). The chromatographic data extracted at four wavelengths (254, 279, 370 and 400 nm) was analyzed individually and at a combination of these wavelengths by the soft independent modeling of class analogies (SIMCA) technique using principal components analysis (PCA) to estimate the separation between the pen samples. Linear discriminant analysis (LDA) measured the probability with which an observation could be assigned to a pen class. The best resolution was obtained by HPLC using data from all four wavelengths together, differentiating 96.4% pen pairs successfully using PCA and 97.9% pen samples by LDA. PCA separated 60.7% of the pen pairs and LDA provided a correct classification of 62.5% of the pens analyzed by IR. The results of this study indicate that HPLC coupled with chemometrics provided a better discrimination of ballpoint pen inks compared to IR. The need to develop a suitable IR method for analysing blue ballpoint pen inks has been emphasized and it is hoped that the development of such a method would indeed provide a valuable tool for the non-destructive analysis of blue ballpoint pen ink samples for forensic purposes. 相似文献
994.
Nilendu PandaNirup B Mondal Sukdeb BanerjeeNiranjan P Sahu Kazuo KoikeTamotsu Nikaido Manuela WeberPeter Luger 《Tetrahedron》2003,59(42):8399-8403
Three new polyhydroxy pregnanes named dregealol (1), volubilogenone (2) and volubilol (3) were isolated from the flowers of Dregea volubilis, and their structures elucidated from extensive 2D NMR analysis. The structure of volubilol (3) was confirmed by X-ray crystallographic studies. The known pregnane derivatives drevogenin D, iso-drevogenin P and 17α-marsdenin were also isolated. 相似文献
995.
微量元素锌在治疗Bell麻痹中的作用 总被引:1,自引:0,他引:1
陈贤雄 《广东微量元素科学》2002,9(3):31-35
为探讨急性早期应用补锌和综合疗法治疗Bell麻痹 ,将 1 5 8例Bell麻痹患者 ,随机分成两组 :(1 )补锌组 (补锌 +综合疗法 ) ;(2 )对照组 (单纯综合疗法 )。对其进行了观察对比治疗 ,同时检测了所有患者治疗前后自身对照发锌值 ,还对所有患者进行了定位诊断、面神经电反应测试、并对面肌功能进行评分。结果表明 ,对定位诊断其病变在D段、面肌功能评分在 1 1分以下、面神经无电反应患者 ,即使给予早期综合治疗 ,效果仍较差 ,而早期给予补锌加综合治疗效果优于对照组 ,其它段内患者治疗次数和治愈天数也均优于对照组。可见微量元素锌在发挥免疫应答、免疫调控中的重要作用 相似文献
996.
卡尔曼滤波紫外光度法同时测定饮料中苯甲酸及糖精的研究 总被引:8,自引:0,他引:8
在酸性条件下,用乙醚萃取、蒸干乙醚后,用NaHCO3溶解残渣,从复杂的样品中分离出苯甲酸和糖精,测定它们在245~281nm之间的紫外吸收,运用卡尔曼滤波算法计算两者的浓度,用新息序列监测干扰物质分离的程度。此法简化了许多分离手续,用于饮料分析,结果满意。 相似文献
997.
Th. Hankemeier P. C. Steketee J. J. Vreuls U. A. Th. Brinkman 《Journal of chromatography. A》1996,750(1-2):161-174
A fully automated at-line solid-phase extraction-gas chromatography procedure has been developed for the analysis of aqueous samples using the PrepStation. The sample extract is transferred from the sample preparation module to the gas chromatograph via an autosampler vial. With flame-ionization detection, limits of determination (S/N=10) of 0.05–0.13 μg/l were obtained for the analysis of HPLC-grade water when modifying the PrepStation by: (i) increasing the sample volume to 50 ml, (ii) increasing the injection volume up to 50 μl, and (iii) decreasing the desorption volume to 300 μl. The HP autosampler had to be modified to enable the automated “at-once” on-column injection of up to 50 μl of sample extract. The amount of packing material in the original cartridge had to be reduced to effect the decrease of the desorption volume. The total set-up did not require any further optimization after having set up the method once. The analytical characteristics of the organonitrogen and organophosphorus test analytes, i.e. recoveries (typically 75–105%), repeatability (2–8%) and linearity (0.09–3.0 μg/l) were satisfactory. The potential of the system was demonstrated by determining triazines and organophosphorus pesticides in river Rhine water at the 0.6 μg/l level using flame-ionization and mass-selective detection. No practical problems were observed during the analysis of more than 100 river water samples. 相似文献
998.
999.
Cheng-Hua DengChuan-Jin Guan Man-Hua ShenCheng-Xue Zhao 《Journal of fluorine chemistry》2002,116(2):109-115
Some newly synthesized fluorinated nitroxides, such as t-butyl perfluoroalkyl nitroxides ButN(O) Rf (Rf=CF3, 5; C2F5, 6; n-C3F7, 7) and s-butyl perfluoroacyl nitroxides BusN(O) CORf (Rf=CF3, 9; n-C3F7, 10) have been employed as ESR probes of solvation in different common organic solvents. In aprotic solvents, the measured aN values for each of the nitroxyl probes show a linear correlation with the cybotactic polar solvent parameters ET (Dimroth) and Z (Kosowar), i.e. aN=bET+c, and aN=b′Z+c′. The physical significance for the slope (b or b′), the slope×ET or slope×Z, the extrapolated intercept on aN axis, c or c′, are linked, respectively, to the sensitivity of a specific nitroxide toward solvation, the magnitude of the overall solvation effect on the aN value, and the intrinsic aN value of each nitroxide in the ideal gaseous state. The intercept on the aN axis may also serve as a new measure of electronegativity for perfluoroalkyl groups, CF3, C2F5, n-C3F7, and perfluoroacyl groups, CF3CO, n-C3F7CO. In protic solvents, i.e. alcohols and carboxylic acids, however, aN values of all the probes, kept almost no change with the increase in ET and Z. Furthermore, the plots of aN versus non-cybotactic solvent constants, such as dipolar moment (μ) and dielectric constant (ε), all show random variations. 相似文献
1000.
《Operations Research Letters》2022,50(1):1-7
Fisher linear discriminant analysis is a well-known technique for dimensionality reduction and classification. The method was first formulated in 1936 by Fisher. In this paper we concentrate on three different formulations of the multi-dimensional problem. We provide a mathematical explanation why two of the formulations are equivalent and prove that this equivalency can be extended to a broader class of objective functions. The second contribution is a rate of convergence of a fixed point method for solving the third model. 相似文献