聚酰胺固相萃取-超高效液相色谱-串联质谱法同时检测饲料中的6种全氟化合物

建立了饲料中6种全氟化合物的聚酰胺固相萃取-超高效液相色谱-串联四极杆质谱分析法。样品采用酸化乙腈提取,在酸性条件下用聚酰胺固相萃取小柱富集,甲醇淋洗净化,5%（v/v）氨水/甲醇溶液洗脱后采用超高效液相色谱-串联四极杆质谱（UPLC-MS/MS）检测。分析柱为Acquity BEH C₁₈（100 mm×2.1 mm,1.7 μm）;流动相为5 mmol/L乙酸铵-乙腈梯度洗脱;在最佳实验条件下,采用多反应监测负离子模式测定,同位素内标法定量。该方法对6种全氟化合物的检出限均小于0.1 μg/kg;对6种饲料及原料的加标回收率为94.2%~108.9%,精密度（RSD）为1.8%~8.6%（n=6）;在0.5~25 μg/L范围内均呈良好的线性关系,线性回归系数r>0.995。该方法前处理成本低,效果好,适合复杂基质样品的检测。     

双波段遥测天线设计

随着航空飞行试验数据量的不断增加,原有IRIG106遥测系统已不能完全适应当前和未来的需求。同时随着网络技术的不断发展,遥测系统的网络化成为新的发展趋势。民用4G通信占用S波段遥测资源使得航空遥测寻找新的传输频段。为了充分利用和保护现有资源,并适应遥测的网络化发展,本文提出在现有S波段遥测基础上增加C波段网络数据传输功能,开展双波段遥测天线设计技术研究。在对天线结构进行合理设计的基础上,提出了一体化馈源设计方案。通过S波段振子与C波段振子的集成化设计,实现了C波段无线网数据与S波段串行数据流的共同传输,极大地提高了遥测数据传输速率,缓解了遥测频率资源紧张的现状。通过飞行试验验证,设计的双波段天线能够满足飞行试验大速率数据的传输需求。     

Determination of macronutrients,micronutrients, non-essential elements in milk based-infant formulas by atomic absorption and inductively coupled plasma-optical emission spectroscopy after microwave and ultrasound assisted digestion

Microwave and ultrasound procedures for samples preparations were adopted and the elements were determined by validated flame atomic absorption and inductively coupled plasma–optical emission spectrometry. Student’s t-test was established whether there was a difference between the sample preparation methods. Trueness of certified values by all methods was ensured which were not differing significantly at 95% level of confidence interval. The highest intensity ratio of magnesium (II)/magnesium (I) was obtained at 1120 radiofrequency value to achieve accurate and reproducible results by inductively coupled plasma–optical emission spectrometry. The value of corresponding correlation coefficient (r²) were obtained as >0.990 indicating the excellent linearity for concentration range chosen for each element to be determined in commercial samples. Results showed that concentrations of calcium, magnesium, potassium, sodium, chromium, copper, iron, manganese, selenium, and zinc found in commercially available products are in good agreement with label as declared by the manufacturers. Exposure to aluminum, cadmium, and lead from consumption of products under evaluation was estimated and it was in compliance with permissible level suggested by European Commission regulations. Regarding the food safety monitoring, the proposed methods are rapid and met green chemistry approach so that can be implemented in laboratories easily for routine analysis.     

FAST望远镜馈源支撑中的力学问题及其研究进展

500 m口径球面射电望远镜FAST拥有多项创新和关键技术,并涉及多个工程学科领域,其中力学在望远镜设备的研制、建设和维护中扮演了非常重要的角色,包括望远镜台址的开挖与支护、反射面系统和馈源支撑系统等的设计均离不开对有关力学问题的分析.本文对十多年来FAST望远镜的馈源支撑系统中与力学方面相关的研究进展进行了全面回顾,重点介绍了当前的研究难点及其有待深入解决的问题.与传统望远镜的刚性馈源支撑相比FAST馈源支撑是一个完全创新的柔性机构,几乎在每一项子系统和机构单元的设计中均存在多种可能的方案设想,需要从中进行优化选择. 从力学角度对每一种方案进行性能评估,为最终的方案优化设计提供合理依据也是当前研究工作的一项紧迫任务.      

Establishment of pressurized liquid extraction followed by HPLC–MS/MS method for the screening of adrenergic drugs,steroids, sedatives,colorants and antioxidants in swine feed

A facile and sensitive multi‐residue detection approach of pressurized liquid extraction following high‐performance liquid chromatography tandem mass spectrometry was established to detect the residues of adrenergic drugs, steroids, sedative, colorant and antioxidant in feed. The conditions employed for pressurized liquid extraction involved acetonitrile/ethyl acetate (1:1, v/v) as the extracting solvent, the temperature 80°C, two cycles and a static time of 10 min. The extraction was followed by a solid‐phase extraction clean‐up step. The separation of samples was done by C₁₈ column with the mobile phase of 5 mM ammonium acetate solution and acetonitrile with 0.1% formic acid. The limits of quantification ranged from 0.03 to 1 μg/kg, limits of detection were in a range of 0.01–0.5 μg/kg, and average recoveries were 70.4–98.6%. The pressurized liquid extraction procedure was optimized and overall method was validated in terms of sensitivity, linearity, selectivity, matrix effect, accuracy, recovery and stability of the target drugs in the pressurized liquid extraction extracts solution. The screening method was proved to be fast, selective, accurate and sensitive for screening drugs.     

超高效液相色谱-电喷雾串联质谱法测定饲料中残留的三聚氰胺

饲料样品经1%三氯乙酸-二甲基亚砜提取,Waters Oasis MCX柱净化,超高效液相色谱分离,最终采用电喷雾串联四极杆质谱进行检测。结果表明,三聚氰胺在饲料中的含量范围为10～5000 μg/kg时,线性关系良好(r＞0.99)。在10～100 μg/kg 的添加水平范围内的平均回收率为83%～94%,相对标准偏差为4.2%～6.5%。该方法的检出限为10 μg/kg。     

L/C双波段高功率微波同轴馈源的辐射特性

 设计了一种高功率微波双波段同轴馈源,从理论分析和数值仿真两方面进行了验证。它采用同轴结构馈电,C波段的工作中心频率为4.15 GHz,利用加入轴向波纹的圆波导结构馈电;L波段的工作中心频率为1.75 GHz,利用同轴波导馈电。通过调整外筒半径的大小,可有效抑制低频段高阶模的传输,同时径向波纹结构可有效改善高频段微波的辐射特性。利用模式匹配法和组合散射矩阵理论对馈源结构进行了分析,理论计算和数值仿真结果具有良好的一致性,所设计的双波段馈源结构紧凑,副瓣电平低,E面和H面方向图等化特性良好。     

Sensitive determination of phenylarsenic compounds based on a dual preconcentration method with capillary electrophoresis/UV detection

A novel method based on off-line hollow fiber based liquid liquid liquid microextraction (HF-LLLME) combined with on-column anion selective exhaustive injection (ASEI)-capillary electrophoresis/ultraviolet (CE/UV) detection was proposed for the speciation of five phenylarsenic compounds including phenylarsonic acid (PAA), 4-aminophenylarsonic acid (4-APAA), 4-hydroxyphenylarsonic acid (4-HPAA), 4-nitrophenylarsonic acid (4-NPAA) and 3-nitro-4-hydroxyphenylarsonic acid (NHPAA) in this paper. In HF-LLLME, the target analytes were extracted from 5 mL aqueous samples (donor solution pH 2.15) through a thin phase of tributyl phosphate (TBP) inside the pores of a polypropylene hollow fiber and finally into an 18 μL 0.8 mmol/L Tris acceptor solution inside the lumen of the hollow fiber. Following HF-LLLME, the acceptor solutions were directly analyzed by ASEI-CE/UV. For ASEI, a large plug of water (91% length of total capillary) was introduced into the separation capillary before sample injection in order to prolong the sample injection time, and thus enhance the stacking efficiency. Under the optimized ASEI conditions, up to 236-fold of enrichment factor (EF) was obtained for the ASEI-CE/UV determination of target phenylarsenic compounds. By combining HF-LLLME with ASEI-CE/UV, EFs ranging from 155 to 1780-fold were achieved and the limits of detection (LODs) (at a signal-to-noise ratio of 3) were in the range of 0.68-6.90 μg/L for five phenylarsenic compounds; the relative standard deviations (RSDs) of corrected peak area were 5.6-11.8%. The proposed HF-LLLME-ASEI-CE/UV method was applied for the determination of five target phenylarsenic compounds in pig feed from a local pig farm, and storage pig litter, soil in agricultural field and lake water collected near this pig farm, the recoveries for the spiked samples were in the range of 85.7-104.5%, 66.7-96.2%, 28.9-46.9% and 86.9-107.8% for pig feed, pig litter, soil and lake water, respectively.     

超宽带匹配馈电结构的设计与实验

设计研制了一种低阻抗传输线向高阻抗超宽带天线馈电的馈电结构,理想情况下,该馈电方法可实现特性阻抗为50Ω的同轴传输线向特性阻抗为200Ω的超宽带天线匹配馈电。分别用TEM喇叭天线和抛物反射面天线进行了实验验证,结果表明,与同轴线直接馈电相比,采用该匹配馈电结构后,TEM喇叭天线的辐射场强提高了15%,反射面天线的辐射场强提高了27%。     

基于相位载波复用的光纤周界安防系统及其实现方法

提出一种利用相位载波的调制解调技术实现白光干涉系统复用的周界安防新方法.该系统在单芯反馈式白光干涉系统的若干感应端,分别串接工作在不同频率的相位调制器.首先利用相位调制技术,将不同干涉子系统的感应端的触发信号从频域上分开|再使用相位解调技术,从同一干涉系统输出信号中获得相应于不同感应端的独立时域信号.实验中通过布设在现场的传感光纤对区域环境振动实现实时记录,用白光干涉方法实现振动信号的提取,利用相位载波复用实现不同区域的定位.理论分析和测试结果表明:通过相位载波复用技术,实现不同传感端共用一套干涉系统的方法,可以显著减小周界安防系统的复杂程度,降低系统成本|该方法能对环境触发信号进行实时监控,并能快速,有效地确定扰动信号的所属区域,具有较高的灵敏度,有利于在大区域,长距离的监控领域获得实施.