Strategies for differentiation of isobaric flavonoids using liquid chromatography coupled to electrospray ionization mass spectrometry

Flavonoids are a class of secondary plant metabolites existing in great variety in nature. Due to this variety, identification can be difficult, especially as overlapping compounds in both chromatographic separations and mass spectrometric detection are common. Methods for distinguishing isobaric flavonoids using MS² and MS³ have been developed. Chromatographic separation of various plant extracts was done with RP‐HPLC and detected with positive ESI‐MS operated in information‐dependent acquisition (IDA) mode. Two methods for the determination of flavonoid identity and substitution pattern, both featuring IDA criteria, were used together with the HPLC equipment. A third method where the collision energy was ramped utilized direct infusion. With the developed strategies, it is possible to differentiate between many isobaric flavonoids. Various classes of flavonoids were found in all of the plant extracts, in the red onion extract 45 components were detected and for 29 of them the aglycone was characterized, while the substituents were tentatively identified for 31 of them. For the strawberry extract, those numbers were 66, 30 and 60, and for the cherry extract 99, 56 and 71. The great variety of flavonoids, several of them isobaric, found in each of the extracts highlights the need for reliable methods for flavonoid characterization. Methods capable of differentiating between most of the isobars analyzed have been developed. Copyright © 2014 John Wiley & Sons, Ltd.     

The assay of pterostilbene in spiked matrices by liquid chromatography tandem mass spectrometry and isotope dilution method

Pterostilbene (trans‐3,5‐dimethoxy‐4‐hydroxystilbene) is an active component found in several plant species, exhibiting important pharmacological properties. A new and reliable method of assaying this phyto compound in various matrices is presented; the assay is based on (1) the selectivity of liquid chromatography (LC) hyphenated with electrospray ionisation (ESI), (2) the specificity of a two‐step mass spectrometric analysis (MS/MS) and (3) the accuracy of the isotope dilution method. The labelled analogue may be conveniently synthesised in a few steps. The sensitivity of the method is confirmed by the very low limit of detection (LOD) and limit of quantitation (LOQ) values achieved in the assay of pterostilbene in two distinct fortified matrices, and is further supported by the observed accuracy values. Copyright © 2010 John Wiley & Sons, Ltd.     

A sensitive quantitative assay for the determination of propafenone and two metabolites, 5‐hydroxypropafenone and N‐depropylpropafenone,in human K2EDTA plasma using LC–MS/MS with ESI operated in positive mode

Propafenone is a potent antiarrhythmic agent; clinically propafenone has been used for a number of cardiac arrhythmias because it possesses multiple modes of action, via beta adrenergic receptor blockade and calcium antagonistic activity. Propafenone (PPF) exhibits extensive saturable presystemic biotransformation (first‐pass effect) resulting in two active metabolites: 5‐hydroxypropafenone (5‐OH PPF) formed by CYP2D6 and N‐ depropylpropafenone (NDP) formed by both CYP3A4 and CYP1A2 enzymes. A specific and sensitive LC–MS/MS method was developed and validated for quantitation of PPF, 5‐OH PPF and NDP using turboion spray in a positive ion mode. A solid‐phase extraction was employed for the extraction from human plasma. Chromatographic separation of analytes was achieved using an ACE‐5 C₈ (50 × 4.6 mm) column with a gradient mobile phase comprising ammonium acetate containing 0.01% TFA in purified water and acetonitrile. The retention times achieved were 1.36, 1.23, 1.24 min and 1.34 min for PPF, 5‐OH PPF, NDP and IS (carbamazepine), respectively. Quantitation was performed by monitoring multiple reaction monitoring transition pairs of m /z 342.30 to m /z 116.20, m /z 358.30 to m /z 116.20, m /z 300.30 to m /z 74.20 and m /z 237.20 to m /z 194.10, respectively. The developed method was validated for various parameters. The calibration curves of PPF and 5‐OH PPF showed linearity from 1 to 500 ng/mL, with a lower limit of quantitation of 1.0 ng/mL and for NDP linearity from 0.1 to 25 ng/mL with a lower limit of quantitation of 0.1 ng/mL. The bias and precision for intra‐ and‐inter batch assays were <10 and 5%, respectively. The developed assay was used to evaluate pharmacokinetic properties of propafenone and its major metabolites in healthy human subjects.     

消防设备电源监控传感模块设计

针对市面上消防设备电源监控传感器采样精度差、通信不稳定、不符合国标规范等设计缺陷,以国家标准GB28184-2011《消防设备电源监控系统》为依据研究设计了一款电流电压型监控传感器。设计创新点在于采用RN8209G芯片进行采样,并通过CAN总线进行通信,在0~50 A电流范围内提高采样精度达到1%。设计产品已通过国标GB28184中4.7节表1中的基础实验及高低温试验要求。     

基于AT89C52的温室用温度监控系统设计

针对目前农业的发展由粗放型向节约型转变的需要,设计一套以AT89C52单片机为核心,与外围器件数字温度传感器DS18B20、数码管、按键、电风扇和加热片共同构成的温度监控系统.该系统能够根据实测温度偏离设定温度值的程度由单片机驱动继电器自动启动相应的加热和降温设备,实现对设定参数的闭环调节,从而将温度保持在恒温,较大程度上节约农业生产人力资源.经实验验证,该系统具有较高的测量精度和控制精度.     

基于嵌入式处理器STM32的抽油机井实时监控系统设计

为了解决抽油机井生产过程中的实时监控问题,本文提出了一种基于嵌入式处理器STM32的抽油机井实时监控系统设计方案,并完成系统的软硬件设计.该系统能够测量抽油机并的油压、油温、三相电流电压、功率、有功、无功、功率因数以及示功图等参数,以此来实现对抽油机井的实时监控.系统各部分与上位机使用RS485总线连接,上位机通过Modbus协议与各模块通信.该系统具有操作简便、测量准确的特点,实现了数据的实时接收和远程监控功能.     

基于LabVIEW的车辆监测系统的设计

基于National Instructionals公司的LabVIEW虚拟仪器技术,设计和搭建了车辆监测系统。利用车载GPS/北斗定位接收系统获取定位信息,通过GPRS将定位信息传递至监控台,监控台将信息汇总后返回至每一车辆,将所有车辆的位置信息共享并显示。监测及显示软件通过LabVIEW编写,以期实现车辆运行状况的实时监控。实验结果表明,该系统能够精确有效地监测和显示车辆的运行状况。     

光纤光栅传感网络的优化研究

光纤光栅传感网络在大型复杂结构健康监测中具有广泛的应用前景,对光纤光栅传感网络优化的研究具有重要的意义。分析了结构健康监测中光纤传感网络优化布局和可靠性的研究现状,对光纤传感网络优化中的传感器优化布局与光纤传感网络可靠性两方面进行研究。通过对结构响应特性研究,提出了对结构静力响应参数监测时,传感器布局的一般规则。将概率计算引入光纤 FBG 传感网络不同拓扑结构,给出了基于不同拓扑结构的光纤传感网络形式及其可靠性数值分析。     

基于ZigBee与安卓的智能远程监控系统的设计

随着中国经济与社会的快速发展,环境监测引起人们的广泛关注。为了解决目前监控系统的不足,设计一种基于ZigBee和因特网的智能远程监控系统。该系统采用TI公司的CC2530芯片及相应传感器构建ZigBee局域网,将采集到的温湿度信息,经过上位机存储并处理,利用因特网或无线移动网络,在安卓智能手机终端上实现数据的远程传输。通过上位机与手机终端,可以查看当前环境状态,保存历史数据,并进行自动报警。给出系统硬件及软件实现方法,包括节点设计、组网流程、数据传输功能、上位机软件设计、安卓智能手机终端软件设计等。实验测试结果说明该系统工作稳定、容易扩展、上位机及手机操作简便。     

环境监测质量管理信息系统的应用研究

互联网环境质量管理信息系统的开发和运用能够有效的为全国环境监测报告提供有力的数据支持,同时完善环境监测质量管理信息系统也是保证加强全国环境监测的基本要求,本文对信息系统在环境监测中的应用进行了研究,希望能够对提高环境质量有所帮助。