一种快速校准GC–MS仪的色谱参数设置方法

介绍一种快速校准GC–MS仪的色谱参数设置方法。该方法进样口温度及传输线温度均设置为280℃,对不同长度的色谱柱采用不同的升温速率(以八氟萘为例15,30 m柱升温速率分别为20,40℃/min)。与校准规范提供的参考方法相比,该方法能节约时间1 h以上,在12台仪器上进行验证测试,八氟萘和硬脂酸甲酯的色谱峰形均较好,且出峰时间分别缩短了13.5,7.75 min(30 m柱)。该方法比校准规范中的参考方法具有更好的适用性,能用于不同型号该类仪器的计量校准。     

毛细管电泳分析中的富集技术及其应用

毛细管电泳（CE）具有分析速度快、分离效率高、样品消耗少、成本低廉等优点,已被应用于无机离子、有机小分子、蛋白质、核酸及细胞等的分析中。CE中最常用的检测方式是紫外检测（UV）,但由于常规进样样品体积小、检测光程短,CE-UV的灵敏度往往不能满足复杂样品中痕量物质直接分析的要求。CE中的在柱富集技术包括堆积、动态pH界面、吹扫和瞬间等速电泳等,可在很大程度上提高CE-UV的检测灵敏度;另外,固相和液相微萃取技术及其与在柱富集技术相结合应用在CE中也能净化样品基质,进一步提高富集倍数,改善分析灵敏度,从而拓宽了CE-UV在复杂样品分析中的应用范围。     

Cloud point extraction combined with electrothermal vaporization inductively coupled plasma mass spectrometry for the speciation of inorganic selenium in environmental water samples

A new method based on cloud point extraction (CPE) separation and electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICPMS) detection has been proposed for the speciation of inorganic selenium in environmental waters. When the temperature of the system is higher than the cloud point temperature (CPT) of the selected surfactant Triton X-114, the complex of Se(IV) with ammonium pyrrolidine dithiocarbamate (APDC) seems to be extracted into the surfactant-rich phase, whereas the Se(VI) remains in aqueous solutions. Thus, an in situ separation of Se(IV) and Se(VI) could be realized. The concentrated analyte was introduced into the ETV-ICP mass spectrometer for determination of Se((IV) after dilution with 200 microL methanol. Se(VI) was reduced to Se(IV) prior to determining total selenium, and its assay was based on subtracting Se(IV) from total selenium. The main factors affecting the CPE and the vaporization behavior of the analyte were investigated in detail. Under the optimized experimental conditions, the limit of detection (LOD) for Se(IV) was 8.0 ng/L with an enhancement factor of 39 when 10 mL of sample solution was preconcentrated to 0.2 mL. The relative standard deviation (RSD) was found to be 3.9% (C(Se(IV)) = 1.0 microg/L, n = 7). The proposed method was applied to the speciation of inorganic selenium in different environmental water samples with the recovery for the spiked samples in the range of 82-102%.     

Porous structure SnSb/amorphous carbon core-shell composite as high capacity anode materials for lithium ion batteries

SnSb/C core-shell powder has been successfully prepared by modified carbothermal reduction method. The shape, size, morphology, and electrochemical properties of the SnSb/C core-shell powder have been investigated. SnSb particles are completely encapsulated by amorphous carbon shell, and the surface of SnSb/C composite has been characterized with porous structure. The composite has a relatively high BET surface area of 253 m²g^?1. The composite exhibits relatively good capacity retention for 50 cycles at a constant current density of 100 mA g^?1 and show excellent rate performance when the current ranges from 50 to 200 mA g^?1. The improvement of reversible capacity and cyclic performance is attributed to loose and amorphous surface structure which could buffer volume variations through cycle process.     

Electrochemical sensor for nitrobenzene based on carbon paste electrode modified with a poly(3,4-ethylenedioxythiophene) and carbon nanotube nanocomposite

A sensitive and selective electrochemical sensor for the determination of nitrobenzene (NB) was developed based on a carbon paste electrode (CPE) modified with a nanocomposite prepared from the conducting polymer poly(3,4-ethylenedioxythiophene) and carbon nanotubes. The modified CPE exhibits good conductivity, a large surface area, and excellent catalytic activity towards the electrochemical reduction of NB. Under optimal conditions, the modified CPE is capable of detecting NB in the 0.25 to 43 μM concentration range and with a detection limit at 83 nM. Moreover, the sensor is highly stable and reusable, and free of interferences by other commonly present nitro compounds. It was used to determine NB in wastewater samples.

H_2SO_4-SiO_2:Highly efficient and novel catalyst for the Ferrier-type glycosylation

<正>Sulfuric acid immobilized on silica gel is designed as a very useful catalyst for synthesis of 2,3-unsaturated glycopyranosides. This handy,metal-free,environment friendly transformation provides high yields andα-stereoselectivities in a very few amount (0.02 eq.) of catalyst and in short reaction times(10 min).     

Synthesis and evaluation of in vitro anticancer activity of novel solasodine derivatives

<正>Solasodine 11 is a steroidal alkaloid with various biological activities.Herein,8 novel solasodine derivatives were synthesized and their effect on prostate cancer cell proliferation was assessed in vitro.Significant improvement in antiproliferative activity was achieved among some of the synthetic analogs.In particular,19 exhibited the most potent inhibitory effect against the proliferation of PC-3 cell line(IC_(50) = 3.91μmol/L).     

溶剂替换法制备氟铃脲水悬浮剂及其分散稳定性

采用溶剂替换法制备了氟铃脲水悬浮剂,通过测定颗粒的平均粒径Dav和颗粒界面的Zeta电位,研究了分散剂种类、添加量以及有机相中乙醇的加入量对水悬浮剂分散稳定性的影响。 结果表明,在相同条件下,以苯乙烯丙烯酸共聚物(MOTAS)作为分散剂制备的水悬浮剂的分散效果较好;当MOTAS添加质量分数为1%时,Dav最小,Zeta电位绝对值最大,体系分散稳定性最好;在有机相中添加乙醇可以显著提高氟铃脲水悬浮剂的分散稳定性,当有机相中乙醇的加入质量分数增加至31.2%时分散稳定性达到最好。     

Synthesis of mono-substituted derivatives of 6-aminoquinoline

Several 6-aminoquinoline derivatives,which could be used in drug design,have been synthesized.The reaction conditions were comparatively studied,and the p-chloroaniline was used as optimum oxidant in Skraup-Doebner-Von Miller reaction.The nitro group was reduced effectively by SnCl₂ with no halo-removed occurred.