超高效液相色谱-串联质谱法测定白芷中51种禁用农药的残留量

将白芷药材粉碎至通过孔径为(250±9.9)μm的网筛,并称取此白芷粉末样品2.00g于聚丙烯管中与水10mL混匀,再加入含1%(体积分数)乙酸的乙腈10.0mL,涡旋1min后加入无水硫酸镁4g和乙酸钠1g,剧烈振荡3min,离心5min,取其上清液5.0mL置于已盛有无水硫酸镁900mg、N-丙基乙二胺(PSA)450mg和硅胶300mg的净化管中,剧烈振荡5min使净化完全,离心5min。移取上清液3.0mL于40℃水浴中减压蒸缩至近干。加入50μg·L^-1的磷酸三苯酯内标溶液300μL,加入乙腈定容至1.0mL,经0.20μm滤膜过滤,取其滤液,按仪器工作条件进行超高效液相色谱-串联质谱法分析。选用Eclipse Plus C18色谱柱和以不同比例的(A)含10mmol·L^-1甲酸铵的0.1%(体积分数)甲酸溶液和(B)乙腈的混合液为流动相,按梯度洗脱程序对白芷中可能残留的51种禁用农药进行色谱分离,并在电喷雾离子源正、负离子(ESI+和ESI-)电离方式和动态多反应监测(dMRM)模式条件下进行串联质谱法测定。采用基质匹配标准曲线法定量。51种农药的质量浓度在一定范围内与其对应的峰面积呈线性关系,并测得其检出限(3S/N)为0.3~5.0μg·kg^-1。标准加入法回收试验的结果显示,其中大部分农药的回收率在71%以上,测定值的相对标准偏差(n=6)均小于20%。按此方法分析了70批白芷样品,共检出16种农药,其中甲拌磷亚砜的检出率达95%,最高检出量为15.2μg·kg^-1;甲拌磷砜和毒死蜱的检出率均为10%,最高检出量依次为3.5,45.0μg·kg^-1,其余13种农药的检出率均低于5%,且检出量均较低。     

利用DPN技术直接构建磁性纳米图形

在纳米尺度下构建有序的磁性模板和图形是当前的研究热点之一 [1,2 ] .这种模板在生物样品的分离[1] 、磁电子学研究和信息存储 [2 ] 等领域具有重要意义 .目前 ,光刻 [3] 、微触点印刷 [4 ] 和自组装 [5] 等多项技术已被用来构建各种纳米模板 .1 999年 ,美国西北大学 Mirkin小组 [6 ]发明的 Dip- pen纳米刻蚀技术 (简称 DPN技术 )更在可控组装方面显示出巨大优越性 .这项技术是在一定驱动力作用下 ,使吸附在原子力显微镜 ( AFM)针尖上的分子“墨水”逐渐转移到基底表面上 ,实现纳米模板的可控构建 .与传统技术相比 ,DPN技术可在纳米尺…     

Optimized Separation of Nine Xanthones by Microemulsion Electrokinetic Chromatography

A microemulsion electrokinetic chromatography method has been firstly used for the separation of the therapeutically important xanthones from Securidaca inappendiculata. The separation of the nine xanthones was systematically optimized with respect to pH, composition of microemulsion,addition of cyclodextrins, applied voltage and column temperature. Baseline separation was successfully achieved for the nine xanthones, which was also compared with that by micellar electrokinetic chromtography.     

纳米晶La_（1－_x）Sr_xFeO_3的合成及气敏特性的研究

用柠檬酸盐法合成出Ｌａ_（１－_ｘ）Ｓｒ_ｘＦｅＯ_３（ｘ＝０．１，０．２，０．３，０．４）原粉，再经固相反应得到纳米晶粉末，用ＴＧ、ＤＴＡ、ＸＲＤ、ＩＲ进行了表征，确证复合氧化物Ｌａ_（１－_ｘ）Ｓｒ_ｘＦｅＯ_３为钙钛矿型结构，粒径在１０～２５ｎｍ之间。实验结果表明，随着固相反应条件不同，产物粒径呈规律性变化．气敏特性研究表明，该纳米晶材料对乙醇有较高的选择性和灵敏度，其选择性顺序为Ｌａ_（０．９）Ｓｒ_（０．１）ＦｅＯ_３＞ＬａＦｅＯ_３＞ＬａＦｅＯ_３（大晶粒）。     

Ce0.8Y0.2O1.9-Ca3(PO4)2-K3PO4复合电解质在中温区的质子导电性及在常压合成氨中的应用

A precursor of Ce_0.8Y_0.2O_1.9(YDC) solid electrolyte was synthesized by the gol-gel method. YDC and phosphates powders were prepared by mixing the YDC and phosphates according to different weight ratios. The mixtures of the YDC and binary phosphates were ground and sintered at 1 400 ℃. The proton conductivity in solid electrolyte of the sintered samples was examined using electrochemical methods at 400～800 ℃. Ammonia was synthesized from nitrogen and hydrogen at atmospheric pressure in the solid state proton conducting cell reactor. The optimal condition for the ammonia production was determined. The result indicated that composite electrolyte of 80wt% YDC: 20wt% binary phosphates as proton conductor could obtain the highest ionic conductivity and ammonia production rate among the four samples, the rate of evolution of ammonia was up to 9.5 × 10^-9 mol·s^-1·cm^-2.     

A New Kind of Void Soap-free P（MMA-EA-MAA） Latex Particles

Soap-flee P(MMA-EA-MAA) particles with narrow size distribution were synthesized by seeded emulsion polymerization of methyl methacrylate (MMA), ethyl acrylate (EA) and methacrylic acid (MAA), and large voids inside the particles were generated by alkali posttreatment in the presence of 2-butanone. Results indicated that the size of void and theparticle volume were related with the amount of 2-butanone. The generation mechanism of voids was proposed.     

多相催化剂的MOVS制备方法

介绍了非均匀相催化剂的ＭＯＶＳ制备方法，以该法制得的ＭｏＯ３催化剂在甲醇选择氧化制甲醛、ＣＯ加氢制高级和喹啉加氢脱氮中均显示出常规催化剂更为优异的催化性能，并探讨了ＭＯＶＳ催化剂的内在特性与催化性能的关系。     

稀土高氯酸盐-谷氨酸配合物[Pr2(L-α-Glu)2(ClO4)(H2O)7](ClO4)3•4H2O的低温热容和热化学研究

合成了一种稀土高氯酸盐-谷氨酸配合物. 经TG/DTG、化学和元素分析、FTIR及与相关文献对比, 确定其组成为[Pr₂(L-α-Glu)₂(ClO₄)(H₂O)₇](ClO₄)₃•4H₂O, 纯度为99.0%以上. 利用显微熔点仪分析发现其没有熔点. 在78～370 K温区, 用精密绝热量热仪测量其低温热容, 在285～306 K温区发现一明显吸热峰, 归结为固-固相变过程. 通过相变温区三次重复热容测量, 得到相变温度T_tr、相变焓Δ_trH_m和相变熵Δ_trS_m分别为(297.158±0.280) K, (12.338±0.016) kJ•mol^－1和(41.520±0.156) J•K^－1•mol^－1. 用最小二乘法将非相变温区的热容对温度进行拟合, 得到了热容随温度变化的两个多项式方程. 用此方程进行数值积分, 得到每隔5 K的舒平热容值和相对于273.15 K的热力学函数值. 根据TG/DTG结果, 推测了该配合物的热分解机理. 依据Hess定律, 选择1 mol•dm^－3盐酸为量热溶剂, 利用等温环境溶解-反应量热计, 测定了该配合物的标准摩尔生成焓为: Δ_fH_m⁰＝－(7223.1±2.4) kJ•mol^－1.     

一种新颖有机-无机杂化配位聚合物[(C10H16N)2（Pb2I6）·2DMF·H2O]n的自组装合成和晶体结构(英)

A novel coordination polymer [(C₁₀H₁₆N)₂（Pb₂I₆）·2DMF·H₂O]_n (C₁₀H₁₆N=N-butyl-2-Methy-Pyridinium) was synthesized by the reaction of Pb(NO₃)₂ with C₆H₁₀NI at room temperature in DMF solvent and structurally characterized by means of X-ray single diffraction. The title compound crystallizes in triclinic system, space group P1 with a=1.1237(2) nm, b=1.25330(16) nm, c=0.808 00(12) nm, α=102.523(4)°, β=92.475(5)°, γ=95.712(10)°, V=1.102 9(3) nm³, Z=1, D_c=2.470 Mg·m^-3, F(000)=738, chemical formula C₂₆H₄₈N₄O₃Pb₂I₆ and M_r=1 640.46, μ（MoKα）=11.849 mm^-1, the final R=0.057 8 and wR=0.166 5 for 3716 observed reflections with I > 2σ(I). The title compound consists of cations ([(C₁₀H₁₆N)⁺] and anion chain(PbI₃^-),they are combined by static attracting forces in the crystal. DMF and H₂O locate between the organic and inorganic moiety. CCDC: 210812.     

水热改性对NiMo/γ-Al2O3加氢脱氮催化剂结构及性能的影响

The influence of hydrothermal modification on the structure and hydrodenitrogenation (HDN) activity of NiMo/γ-Al₂O₃catalyst was studied in the range 140～180 ℃. The experimental results indicated that the hydrodenitrogenation reaction rate of pyridine was accelerated using the NiMo/γ-Al₂O₃catalyst synthesized via hydrothermal route due to the change of the structure, the increase of the amount of Mo and Ni and the rise of the specific surface area. The change of the structure of catalysts was enhanced at higher hydrothermal temperature, producing NiMo/γ-Al₂O₃catalyst with better HDN activity.