Development and validation of an analytical methodology for the determination of p,p′-DDT, p,p′-DDE and p,p′-DDD in fish oil pills

An analytical methodology was proposed and validated to be applied to the determination of p,p′-DDT and its metabolites p,p′-DDE and p,p′-DDD in fish oil. The analytical procedure presented in this paper involves a single-step clean up process prior to the analysis. A solution of 1,2,3,4-tetrachloronaphtalene was used as internal standard.The analytical technique used was gas chromatography coupled to an electron capture detector. Details on the validation process are provided.The limits of detection ranged from 2.6 to 4.7 pg μL^− 1. The BCR 598 standard reference material (cod liver oil) was used to evaluate the performance of the methodology with satisfactory recoveries for all the compounds.The analytes were determined in three different fish oil pills sold in Spain as a supplementary vitamin support. The sum of p,p′-DDT and metabolites was from 13.2 to 51.3 ng g^− 1, the dominant compound being p,p′-DDE.     

端视式全谱直读电感耦合等离子体发射光谱法测定高纯氧化镧中稀土杂质

电感耦合等离子体发射光谱(ICP-AES)测定高纯氧化镧中14个稀土元素杂质,镧对其它稀土元素的光谱干扰比较严重,要求光谱仪单色器有较高的分辨率。使用端视式全谱直读ICP-AES仪,选择测定波长,工作参数优化,讨论了镧和酸度的影响。大部分稀土元素测定使用曲线拟合(FACT)的背景校正方法。该方法的稀土元素氧化物检出限达到3×10-4~0.022 mg.L-1(3σ)。     

Applications of a miniaturized fluorimetric photodiode array detector for capillary liquid chromatography

A high sensitivity, multichannel fluorescence detector with small volume has been developed for capillary column liquid chromatography. Using an intensified linear photodiode array to monitor fluorescence emission, several important mixtures exhibiting native fluorescence have been examined following high efficiency separation on a capillary column. By correlating mass spectral, fluorescence spectral, and retention time data, information of potential utility in the structural elucidation of aromatic molecules contained in complex mixtures can be obtained. Examples include the separation and spectral examination of the polyaromatic compounds in samples of both biological and environmental interest.     

Fermentation characteristics and the dynamic trend of chemical components during fermentation of Massa Medicata Fermentata

As a representative of traditionally fermented Chinese medicine, Massa Medicata Fermentata (MMF) shows the functions of invigorating the spleen and stomach and promoting digestion, which plays an important role in the treatment of gastrointestinal diseases. The fermentation mechanism and the key factors that affect the quality of MMF have not been revealed yet, which has become an urgent issue that limits its clinical application. This article aims to systematically and comprehensively reveal the transformation of physical properties and the dynamic trend of chemical components including substrate components, volatile components, and lactic acid as anaerobic fermentation product during MMF fermentation. Along with obvious hyphae growth observed for MMF, the weight of MMF decreased, and the moisture and temperature increased. Through the quantified 14 components from substrate, ferulic acid increased from 45.53 ± 6.94 to 141.89 ± 78.40 μg/g, while glycosides and phenolic acids declined except caffeic acid. Also, within the 66 volatile components analyzed, alcohols and acids increased, while aldehydes and ketones decreased. Lactic acid was not detected in the fermentation substrate, but an apparent increase in lactic acid content was observed along with the increased fermentation days, resulting in 2.54 ± 0.15 mg/g on day 8. Based on the tested components, the fermentation process of MMF was discriminated into three distinct stages by principal component analysis, and an optimal fermentation time of four days was proposed. The results of this study will be of great significance to clarify the characteristics of fermentation and conduce to improving quality standards of MMF.     

用于高能物理实验电子读出芯片的低噪声锁相环芯片设计

基于TSMC 180 nm工艺设计并流片测试了一款用于高能物理实验的电子读出系统的低噪声、低功耗锁相环芯片。该芯片主要由鉴频鉴相器、电荷泵、环路滤波器、压控振荡器和分频器等子模块组成,在锁相环电荷泵模块中,使用共源共栅电流镜结构精准镜像电流以减小电流失配和用运放钳位电压进一步减小相位噪声。测试结果表明,该锁相环芯片在1.8 V电源电压、输入50 MHz参考时钟条件下,可稳定输出200 MHz的差分时钟信号,时钟均方根抖动为2.26 ps(0.45 mUI),相位噪声在1 MHz频偏处为-105.83 dBc/Hz。芯片整体功耗实测为23.4 mW,锁相环核心功耗为2.02 mW。     

Ka频段高灵敏度检波器研制

介绍了一种高电压灵敏度、低切线灵敏度检波器的设计方法。在建立检波二极管简化物理模型的基础上,进行了检波二极管Ka频段阻抗参数的提取,再根据提取的阻抗参数,通过仿真优化了射频匹配网络,使得检波器能够较好地工作在23～34 GHz。实测表明,在1.2 kHz视频带宽下,当输入功率为-30 dBm时,23～34 GHz范围内电压灵敏度高于6 000 mV/mW,切线灵敏度优于-56 dBm,对应等效噪声功率(Noise Equivalent Power, NEP)估算为11.5～36 pW/Hz^1/2。对比实测与仿真结果较为一致,证明了阻抗参数提取的有效性。     

引入自上向下特征融合的小目标检测算法

针对原始SSD(Single Shot Multibox Detector)算法未充分利用各特征层之间关系导致浅层特征层缺乏小目标语义信息的问题,为了提高对小目标的检测能力,提出了一种结合PANet多尺度特征融合网络和自上向下特征融合路径的TTB-SSD(Top to Bottom SSD)改进算法。首先,使用PANet多尺度特征融合网络对特征进行反复提取,从而获得丰富的多尺度语义信息;然后,使用一种深层特征融合模块将浅层特征层的空间信息传递到深层特征层,进而更准确地对小目标进行定位;最后,为了增强浅层特征层的语义信息,构造了自上向下的特征融合路径,从而强化浅层对小目标检测的准确率。实验结果表明,在PASCAL VOC2007测试集检测的mAP(Mean Average Precision)值达到80.5%,对目标的mAP较原始SSD提高了5.7%,证明了该算法对小目标检测的有效性。     

位置敏感探测器光斑脱靶误差补偿方法研究

为了提高位置敏感探测器(PSD)的位置检测范围,解决光斑在探测器光敏面脱靶时无法准确定位光斑的问题,提出一种光斑脱靶误差补偿方法,分析了脱靶前后PSD检测光斑能量重心变化规律,建立了PSD光强信号与位置检测误差间的函数关系。实验结果表明:当PSD光敏面尺寸为12mm×12mm时,对于半径为5mm的高斯光斑,通过所提出的光斑补偿方案补偿后PSD的X轴检测范围提高了66.7%,位置检测平均相对误差不超过5%,该方法对提高PSD位置检测性能具有重要的意义。     

Analytical Detectors Based on Microplasma Spectrometry

Miniaturizing all dimensions of apparatus, such as electronics and computers, is the current trend followed by scientists in various fields. The idea of Lab-on-a-Chip has significantly expanded and found its broad applications in analytical chemistry. Microplasmas can act as a sample excitation source and are the miniaturized versions of full-sized plasmas. These can be created in various forms, such as direct current, microwave induced, capacitively coupled and inductively coupled plasmas. Scaling down the size would reduce the amount of gases, liquids and consumables required, as well as the sample analysis time, which in turn would decrease the operating costs. Therefore, several research groups are involved in the development of microplasmas for utilisation in analytical instruments.     

The effect of capillary column diameter on the performance of thermal conductivity detectors

The concentration sensitivity of a thermal conductivity detector (TCD) depends, among other factors, on the amount of sample mixture in the detector's sensing cell. Since the cell volume has to be appropriately matched with column diameter, it makes the concentration sensitivity of a TCD dependent on column diameter and, therefore, on the speed of gas chromatography. Through reduction of column diameter, higher speed tends to lead to a reduction in the concentration sensitivity of the cell. The factor which the most directly affects the concentration sensitivity of a TCD cell is the heat power conducted through the cell. The higher the power, the greater the sensitivity. The limit of detection of a TCD depends on the concentration-sensitivity of its cell and on the level of statistical errors in the measurement. The errors increase with increasing analysis speed. As the column diameter is reduced, the errors cause additional worsening (on top of the decrease in concentration sensitivity) of the detection limit, dynamic range, and other performance characteristics of the TCD.