HPLC-APCI-MS determination of free fatty acids in Tibet folk medicine Lomatogonium rotatum with fluorescence detection and mass spectrometric identification

A simple and sensitive method for the determination of free fatty acids (FFAs) using acridone-9-ethyl-p-toluenesulfonate (AETS) as a fluorescence derivatization reagent by high performance liquid chromatography (HPLC) has been developed. Free fatty acid derivatives were separated on an Eclipse XDB-C-8 column with a good baseline resolution and detected with the fluorescence of which excitation and emission wavelengths of derivatives were set at lambda(ex) 404 and lambda(em) 440 nm, respectively. Identification of 19 fatty acid derivatives was carried out by online post-column mass spectrometry with an atmospheric pressure chemical ionization (APCI) source under positive-ion detection mode. Nineteen FFAs from the extract of Lomatogonium rotatum are sensitively determined. The results indicate that the plant Lomatogonium rotatum is enriched with an abundance of FFAs and FFAs of higher contents, which mainly focus on even carbon atoms, C-14, C-16, and C-18. The validation of the method including linearity, repeatability, and detection limits was examined. Most linear correlation coefficients for fatty acid derivatives are > 0.9989, and detection limits (at signal-to-noise of 3: 1) are 12.3-43.7 fmol. The relative standard deviations (RSDs) of the peak areas and retention times for 19 FFAs standards are < 2.24% and 0.45%, respectively. The established method is rapid and reproducible for the separation determination of FFAs from the extract of Lomatogonium rotatum with satisfactory results.

2-(2-Phenyl-1H-phenanthro-[9,10-d]imidazole-1-yl)-acetic acid (PPIA) and its application for determination of amines by high performance liquid chromatography with fluorescence detection and identification with mass spectroscopy/atmospheric pressure chemical ionization

A simple, sensitive, and mild method for the determination of amino compounds based on a condensation reaction with 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC-HCI) as the dehydrant with fluorescence detection has been developed. Amines were derivatized to their acidamides with labeling reagent 2-(2-phenyl-1H-phenanthro-[9,10-d]imidazole-1-yl)-acetic acid (PPIA). Studies on derivatization conditions indicated that the coupling reaction proceeded rapidly and smoothly in the presence of a base catalyst in acetonitrile to give the corresponding sensitively fluorescent derivatives with an excitation maximum at lambda(ex) 260nm and an emission maximum at lambda(em) 380nm. The labeled derivatives exhibited high stability and were enough to be efficiently analyzed by high-performance liquid chromatography. Identification of derivatives was carried out by online post-column mass spectrometry (LC/APCI-MS/MS) and showed an intense protonated molecular ion corresponding m/z [MH](+) under APCI in positive-ion mode. At the same time, the fluorescence properties of derivatives in various solvents or at different temperature were investigated. The method, in conjunction with a gradient elution, offered a baseline resolution of the common amine derivatives on a reversed-phase Eclipse XDB-C-8 column. LC separation for the derivatized amines showed good reproducibility with acetonitrile-water as mobile phase. Detection limits calculated from 0.78 pmol injection, at a signal-to-noise ratio of 3, were 3.1-18.2 fmol. The mean intra- and inter-assay precision for all amine levels were < 3.85% and 2.11%, respectively. Excellent linear responses were observed with coefficients of > 0.9996. The established method for the determination of aliphatic amines from real wastewater and biological samples was satisfactory. (c) 2006 Elsevier B.V. All rights reserved.

Development of a sensitive fluorescent derivatization reagent 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC) and its application for determination of amino acids from seeds and bryophyte plants using high-performance liquid chromatography with fluorescence detection and identification with electrospray ionization mass spectrometry

A pre-column derivatization method for the sensitive determination of amino acids and peptides using the tagging reagent 1,2-benzo-3,4dihydrocarbazole-9-ethyl chloroformate (BCEOC) followed by high-performance liquid chromatography with fluorescence detection has been developed. Identification of derivatives was carried out by liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS/MS). The chromophore of 2-(9-carbazole)-ethyl chloroformate (CEOC) reagent was replaced by 1,2-benzo-3,4-dihydrocarbazole functional group, which resulted in a sensitive fluorescence derivatizing reagent BCEOC. BCEOC can easily and quickly label peptides and amino acids. Derivatives are stable enough to be efficiently analyzed by high-performance liquid chromatography. The derivatives showed an intense protonated molecular ion corresponding m/z (M + H)(+) under electrospray ionization (ESI) positive-ion mode with an exception being Tyr detected at negative mode. The collision-induced dissociation of protonated molecular ion formed a product at m/z 246.2 corresponding to the cleavage of C-O bond of BCEOC molecule. Studies on derivatization demonstrate excellent derivative yields over the pH 9.0-10.0. Maximal yields close to 100% are observed with a 3-4-fold molar reagent excess. Derivatives exhibit strong fluorescence and extracted detzvatization solution with n-hexane/ethyl acetate (10:1, v/v) allows for the direct injection with no significant interference from the major fluorescent reagent degradation by-products, such as 1,2-benzo-3,4-dihydrocarbazole-9-ethanol (BDC-OH) (a major by-product), mono- 1,2-benzo-3,4-dihydrocarbazole-9-ethyl carbonate (BCEOC-OH) and bis-(1,2-benzo-3,4-dihydrocarbazole-9-ethyl) carbonate (BCEOC)(2). In addition, the detection responses for BCEOC derivatives are compared to those obtained with previously synthesized 2-(9-carbazole)-ethyl chloroformate (CEOC) in our laboratory. The ratios AC(BCEOC)/AC(CEOC) = 2.05-6.51 for fluorescence responses are observed (here, AC is relative fluorescence response). Separation of the derivatized peptides and amino acids had been optimized on Hypersil BDS C-18 column. Detection limits were calculated from 1.0 pmol injection at a signal-to-noise ratio of 3, and were 6.3 (Lys)-177.6 (His) fmol. The mean interday accuracy ranged from 92 to 106% for fluorescence detection with mean %CV < 7.5. The mean interday precision for all standards was < 10% of the expected concentration. Excellent linear responses were observed with coefficients of > 0.9999. Good compositional data could be obtained from the analysis of derivatized protein hydrolysates containing as little as 50.5 ng of sample. Therefore, the facile BCEOC derivatization coupled with mass spectrometry allowed the development of a highly sensitive and specific method for the quantitative analysis of trace levels of amino acids and peptides from biological and natural environmental samples. (c) 2005 Elsevier B.V. All rights reserved.

旋翼飞行机器人故障诊断与容错控制技术综述

对故障诊断和容错技术的发展过程进行了简要概述,以旋翼飞行机器人为研究对象,在分析了旋翼飞行机器人故障诊断与容错控制特点的基础上,介绍了当前国内外在该领域的研究进展和主要方法.最后,总结了该领域待解决的难点问题,并指出了该研究领域的发展趋势.

ROV推进系统故障检测及容错控制研究

遥控水下机器人( ROV )工作在未知的不确定的复杂海洋环境中，其机械部件和控制系统极易出现故障。推进器是ROV的动力装置，对ROV完成水下作业，顺利回收起着至关重要的作用。推进器经常受到水草、异物的干扰而损坏，同时其内部的机械和电子组件也因老化、发热、受力而容易损坏，因此推进系统故障是ROV经常发生的故障之一。故障检测是提高其推进系统可靠性的重要环节，为ROV的容错控制和紧急回收等应急措施提供科学依据。ROV的容错控制对提高ROV的可靠性和机动性有着重要的意义。 针对ROV推进系统的特点，本文研究了ROV推进系统的系统辨识，故障检测和容错控制问题。 本文给出了一种基于控制量输入的ROV模型辨识方法，减小了辨识的工作量。该模型以螺旋桨驱动电机的电压控制量为输入，以各个自由度的运动状态为输出，不需进行螺旋桨推力标定。针对这种辨识方式，本文给出一种ROV系统辨识的非线性模型和简化的线性模型，对于相应的模型设计了辨识方法。通过实验验证了模型和方法的有效性。 针对ROV的故障检测问题，给出基于模型与推进电机电流的故障检测方法，设计了故障检测策略，实现对故障的分离和定位。通过模拟故障实验验证了方法的有效性。 针对ROV推进系统容错控制分配问题，本文提出了基于SVD分解(奇异值分解)与定点分配的混合算法。与传统的方法相比，它回避了求伪逆矩阵的问题，减小了计算量；能够满足推进器饱和约束限制。利用水下实验平台的推进系统模型进行了仿真实验，验证了算法的正确性和有效性。

Phage M13Ko7 Detection With Biosensor Based On Imaging Ellipsometry And Afm Microscopic Confirmation

A rapid detection and identification of pathogens is important for minimizing transfer and spread of disease. A label-free and multiplex biosensor based on imaging ellipsometry (BIE) had been developed for the detection of phage M13KO7. The surface of silicon wafer is modified with aldehyde, and proteins can be patterned homogeneously and simultaneously on the surface of silicon wafer in an array format by a microfluidic system. Avidin is immobilized on the surface for biotin-anti-M13 immobilization by means of interaction between avidin and biotin, which will serve as ligand against phage M13KO7. Phages M13KO7 are specifically captured by the ligand when phage M13KO7 solution passes over the surface, resulting in a significant increase of mass surface concentration of the anti-M13 binding phage M13KO7 layer, which could be detected by imaging ellipsometry with a sensitivity of 10(9) pfu/ml. Moreover, atomic force microscopy is also used to confirm the fact that phage M13KO7 has been directly captured by ligands on the surface. It indicates that BIE is competent for direct detection of phage M13KO7 and has potential in the field of virus detection. (C) 2008 Elsevier B.V. All rights reserved.

Ground target detection, classification and sensor fusion in distributed fiber seismic sensor network - art. no. 683015

This paper describes the ground target detection, classification and sensor fusion problems in distributed fiber seismic sensor network. Compared with conventional piezoelectric seismic sensor used in UGS, fiber optic sensor has advantages of high sensitivity and resistance to electromagnetic disturbance. We have developed a fiber seismic sensor network for target detection and classification. However, ground target recognition based on seismic sensor is a very challenging problem because of the non-stationary characteristic of seismic signal and complicated real life application environment. To solve these difficulties, we study robust feature extraction and classification algorithms adapted to fiber sensor network. An united multi-feature (UMF) method is used. An adaptive threshold detection algorithm is proposed to minimize the false alarm rate. Three kinds of targets comprise personnel, wheeled vehicle and tracked vehicle are concerned in the system. The classification simulation result shows that the SVM classifier outperforms the GMM and BPNN. The sensor fusion method based on D-S evidence theory is discussed to fully utilize information of fiber sensor array and improve overall performance of the system. A field experiment is organized to test the performance of fiber sensor network and gather real signal of targets for classification testing.

Sensitive and Rapid Detection of Genetic Modified Soybean (Roundup Ready) by Loop-Mediated Isothermal Amplification

Using the LAMP method, a highly specific and sensitive detection system for genetically modified soybean (Roundup Ready) was designed. In this detection system, a set of four primers was designed by targeting the exogenous 35S epsps gene. Target DNA was amplified and visualized on agarose gel within 45 min under isothermal conditions at 65 degrees C. Without gel electrophoresis, the LAMP amplicon was visualized directly in the reaction tube by the addition of SYBR Green I for naked-eye inspection. The detection sensitivity of LAMP was 10-fold higher than the nested PCR established in our laboratory. Moreover, the LAMP method was much quicker, taking only 70 min, as compared with 300 min for nested PCR to complete the analysis of the GM soybean. Compared with traditional PCR approaches, the LAMP procedure is faster and more sensitive, and there is no need for a special PCR machine or electrophoresis equipment. Hence, this method can be a very useful tool for GMO detection and is particularly convenient for fast screening.

Elliptic Object Detection Based on Shape Preserving and Active Contour

本文通过形状约束方程(组)与一般主动轮廓模型结合,将目标形状与主动轮廓模型融合到统一能量泛函模型中,提出了一种形状保持主动轮廓模型即曲线在演化过程中保持为某一类特定形状。模型通过参数化水平集函数的零水平集控制演化曲线形状,不仅达到了分割即目标的目的,而且能够给出特定目标的定量描述。根据形状保持主动轮廓模型,建立了一个用于椭圆状目标检测的统一能量泛函模型,导出了相应的Euler-Lagrange常微分方程并用水平集方法实现了椭圆状目标检测。此模型可以应用于眼底乳头分割,虹膜检测及相机标定。实验结果表明,此模型不仅能够准确的检测出给定图像中的椭圆状目标,而且有很强的抗噪、抗变形及遮挡性能。