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131.
Benturquia N Couderc F Sauvinet V Orset C Parrot S Bayle C Renaud B Denoroy L 《Electrophoresis》2005,26(6):1071-1079
Serotonin or 5-hydroxytryptamine (5-HT) is a major neurotransmitter in the central nervous system. In this work, a method for analyzing 5-HT in brain microdialysis samples using a commercially available capillary electrophoresis (CE) system has been developed. A pH-mediated in-capillary preconcentration of samples was performed, and after separation by capillary zone electrophoresis, native fluorescence of 5-HT was detected by a 266 nm solid-state laser. The separation conditions for the analysis of 5-HT in standard solutions and microdialysates have been optimized, and this method has been validated on both pharmacological and analytical bases. Separation of 5-HT was performed using a 80 mmol/L citrate buffer, pH 2.5, containing 20 mmol/L hydroxypropyl-beta-cyclodextrin (HP-beta-CD) and +30 kV voltage. The detection limit was 2.5 x 10(-10) mol/L. This method allows the in vivo brain monitoring of 5-HT using a simple, accurate CE measurement in underivatized microdialysis samples. 相似文献
132.
The separation and detection of commonly used preservatives (benzoate, sorbate) and vitamin C by both conventional CE and microchip electrophoresis with capacitively coupled contactless conductivity detection is presented. The separation was optimized by adjusting the pH-value of the buffer and the use of hydroxypropyl-beta-CD (HP-beta-CD) and CTAB as additives. For conventional CE, optimal separation conditions were achieved in a histidine/tartrate buffer at pH 6.5, containing 0.025% HP-beta-CD and 0.1 mM CTAB. LOD ranged from 0.5 to 3 mg/L (S/N = 3) and the RSDs for migration time and peak area were less than 0.1 and 2%, respectively. A considerable reduction of analysis time can be accomplished by using microchip electrophoresis without significant loss in sensitivity under optimal separation conditions. A histidine/tartrate buffer at pH 6.5, incorporating 0.06% HP-beta-CD and 0.25 mM CTAB, gave detection limits ranging between 3 and 10 mg/L and satisfactory reproducibilities of < or =0.4% for the migration time and < or =3.5% for the peak area. The methods developed are useful for the quantitative determination of food additives in real samples such as soft drinks and vitamin C tablets. 相似文献
133.
Capillary GC coupled to an atomic emission detector (AED) provides a powerful new hyphenated technique for the separation and characterization of complex mixtures and compounds. The AED provides simultaneous and truly specific multi-element detection. The specificity of detection reduces the need for the complex sample pretreatment procedures which are necessary to reduce the interference from co-eluted substances which is experienced with detectors such as the FID and the ECD. A range of environmentally significant problems has been studied, including PCB analysis, the characterization of the reaction products of a novel waste treatment process, and the profiling of sulfur-containing species formed by the pyrolysis of various types of coal. 相似文献
134.
Summary Retention models for ionic compounds in reversed-phase ion-pair chromatographic systems have been developed on the basis of
the capacity ratios of solutes and ionic mobile phase components using indirect detection. The binding to the adsorbent, μBondapak
Phenyl, has been expressed by ion-pair distribution constants and tested in the retention models by non-linear regression.
All the ionic compounds followed adsorption models of the Langmuir type comprising two kinds of binding sites with widely
different adsorption capacities and binding constants. The results indicate certain differences between the two sites regarding
the binding of cationic and anionic components, respectively. 相似文献
135.
Summary The distribution equilibria of cationic compounds in reversed-phase chromatographic systems (ion-pair chromatography) have
been studied on the basis of their effect on a detectable mobile phase component. The solid phase was a polystyrene-divinylbenzene
copolymer and the detectable component, a quaternary ammonium ion, 1-methylpyridine. The solutes were mono- and divalent amines
and quaternary ammonium ions.
The cations can be retained by ion-pair adsorption and ion exchange. Expressions for the ion-pair retention of the solutes
and the mobile phase cation (system peak) have been developed assuming Langmuir distribution of ion pairs to a solid phase
with one kind of binding site. The validity of the expressions has been tested by evaluation of ion-pair distribution constants
using non-linear curve fitting techniques. Good agreement for the constants of common ion pairs was obtained from different
kinds of capacity ratio expressions.
Ion exchange retention can appear beside ion-pair retention, and it has been observed in the pH range 1.6–6.1. The effect
depends not only on cations in the mobile phase, but also on the nature of the buffering systems. 相似文献
136.
Summary Conditions have been established for identification and quantification of cefuroxime axetil and cefuroxime by thin-layer chromatography and densitometry. Good separation of these compounds was achieved on silica gel by use of chloroform–ethyl acetate–glacial acetic acid–water, 4:4:4:1 (v/v), as mobile phase. UV densitometry was used to detect spots on chromatograms. Under these conditions the limits of detection for cefuroxime axetil and cefuroxime were 40 ng and 30 ng, respectively. Recoveries of cefuroxime axetil and cefuroxime were 99.93% and 97.94%, respectively. 相似文献
137.
138.
中药材重金属元素快速检测对污染监控及人们健康具有重要意义。激光诱导击穿光谱技术(Laser Induced Breakdown Spectroscopy, LIBS)属于一种快速检测方法,研磨压片等预处理方法相对样品消解已有所简化,但破坏了样品的物理性质,且不能满足中药材大宗品种、大批量检测需求。若进一步简化样品预处理,将更加凸显LIBS快速检测的优势。本文建立了激光诱导击穿光谱技术(LIBS)快速微损检测中药材样品重金属元素定标方法。线性相关系数R2为0.7764,建立的微损定标曲线线性可用于切片党参LIBS快速检测,对待测党参切片样品检测平均相对误差为3.74%,与电感耦合等离子体质谱法(ICP-MS)对比,相关系数R2为0.7957,验证了LIBS技术微损检测的可行性。制备的党参参考定标样品可多次重复用于待测样定标和仪器标定等。实验对待测党参样品仅进行切片处理,避免了研磨、压片等预处理,更加充分地体现LIBS快速检测的优势,为LIBS技术应用于中药材重金属元素快检等领域提供了一种新方法。 相似文献
139.
140.
State-of-the-art speech watermarking techniques enable speech signals to be authenticated and protected against any malicious attack to ensure secure speech communication. In general, reliable speech watermarking methods must satisfy four requirements: inaudibility, robustness, blind-detectability, and confidentiality. We previously proposed a method of non-blind speech watermarking based on direct spread spectrum (DSS) using a linear prediction (LP) scheme to solve the first two issues (inaudibility and robustness) due to distortion by spread spectrum. This method not only effectively embeds watermarks with small distortion but also has the same robustness as the DSS method. There are, however, two remaining issues with blind-detectability and confidentiality. In this work, we attempt to resolve these issues by developing an approach called the LP-DSS scheme, which takes two forms of data embedding for blind detection and frame synchronization. We incorporate blind detection with frame synchronization into the scheme to satisfy blind-detectability and incorporate two forms of data embedding process, front-side and back-side embedding for blind detection and frame synchronization, to satisfy confidentiality. We evaluated these improved processes by carrying out four objective tests (PESQ, LSD, Bit-error-rate, and accuracy of frame synchronization) to determine whether inaudibility and blind-detectability could be satisfied. We also evaluated all combinations with the two forms of data embedding for blind detection with frame synchronization by carrying out BER tests to determine whether confidentiality could be satisfied. Finally, we comparatively evaluated the proposed method by carrying out ten robustness tests against various processing and attacks. Our findings showed that an inaudible, robust, blindly detectable, and confidential speech watermarking method based on the proposed LP-DSS scheme could be achieved. 相似文献