An efficient method to synthesize TNAD by the nitration of 1,4,5,8- tetraazabicyclo-[4,4,0]-decane with N20s and acidic ionic liquids

An experimental study was carried out on the direct nitration of 1,4,5,8-tetraaza-bicyclo-[4,4,0]-decane to synthesize 1,4,5,8-tetranitro-1,4,5,8-tetraazabicyclo-[4,4,0]-decane(TNAD) with N2O5 catalyzed by acidic ionic liquids. Various ionic liquids, such as [HMim]X, [(CH2)4SO3HMim]X and [Capl]X(X = pTSO, NO3, HSO4), and various parameters such as equivalents of ionic liquid, molar ratio of N2O5 to the starting material, reaction time and temperature, and solvent were investigated. Ionic liquid [(CH2)4SO3HMim]HSO4 showed better catalytic activity. In the presence of 3% molar ratio of [(CH2)4SO3HMim]HSO4 ionic liquid to the staring material, the yield of 1,4,5,8-tetranitro-1,4,5,8-tetraazabicyclo-[4,4,0]-decane was improved by 6.2% compared to the system without ionic liquid.     

Graphene oxide assisted facile hydrothermal synthesis of LiMn0.6Fe0.4PO4 nanoparticles as cathode material for lithium ion battery

Assisted by graphene oxide（GO）,nano-sized LiMn0.6Fe0.4PO4 with excellent electrochemical performance was prepared by a facile hydrothermal method as cathode material for lithium ion battery.SEM and TEM images indicate that the particle size of LiMn0.6Fe0.4PO4（S2）was about 80 nm in diameter.The discharge capacity of LiMn0.6Fe0.4PO4 nanoparticles was 140.3 mAh-g^1 in the first cycle.It showed that graphene oxide was able to restrict the growth of LiMn0.6Fe0.4PO4 and it in situ reduction of GO could improve the electrical conductivity of LiMn0.6Fe0.4PO4 material.     

荧光增强型量子点探针检测痕量谷氨酸脱氢酶

建立了荧光增强型量子点探针检测痕量谷氨酸脱氢酶(GLDH)的方法,GLDH是种烟酰胺腺嘌呤二核苷酸(NAD+)依赖的酶分子,具有氧化性的NAD+通过电子转移淬灭CdTe量子点的荧光,而GLDH催化的生物化学反应可以消耗NAD+。在所采用的NAD+/GLDH体系中,量子点的荧光先被NAD+淬灭,加入GLDH消耗NAD+,荧光会因NAD+的减少而增强。利用这种高选择性的酶促反应可以检测浓度范围比较宽的GLDH(10~1000 U/L)。对于这个浓度范围GLDH的检测在临床上有重要意义,可用于诊断不同类型的肝脏疾病。     

液相色谱-串联质谱法同时检测DNA中3-甲基腺嘌呤和3-乙基腺嘌呤

利用阳离子交换固相萃取柱(Waters Oasis MCX)富集净化DNA样品,建立了液相色谱串联质谱(LC-MS/MS)同时检测DNA中3-甲基腺嘌呤(N3-MeA)和3-乙基腺嘌呤(N3-EtA)的方法。采用氘代-3-甲基腺嘌呤(d3-N3-MeA)和氘代-3-乙基腺嘌呤(d5-N3-EtA)为内标;进样量3μL,分析时间为13 min;亲水相互作用色谱柱(Waters XBridge HILIC)进行液相分离,流动相为10 mmol/L甲酸铵-乙腈溶液(5∶95,V/V,pH=4.0),流速250μL/min;质谱条件:电喷雾离子源,多反应监测正离子扫描方式;电喷雾电压:5500 V,雾化气:369 Pa,气帘气:185 Pa,电离温度:400℃,驻留时间:40 ms。本方法对N3-MeA和N3-EtA的检出限分别为0.043和0.007μg/L,方法回收率为87.8%~103.0%。采用本方法检测了卷烟烟气粒相物暴露的DNA中N3-MeA和N3-EtA含量。结果表明,卷烟烟气粒相物暴露后的小牛胸腺DNA中3-甲基腺嘌呤和3-乙基腺嘌呤可被本方法定量检出。     

二氧化硅-氧化石墨烯复合物固相萃取-高效液相色谱法检测植物油中黄曲霉毒素B1、B2

以二氧化硅-氧化石墨烯复合物为固相萃取材料,建立了植物油中黄曲霉毒素B1、B2的高效液相色谱(HPLC)检测方法。优化的条件为:复合材料的最佳用量为0.15 g,最佳萃取时间20 min,洗脱溶剂为乙腈,洗脱次数为2次。结果表明,在优化条件下,建立的二氧化硅-氧化石墨烯复合物固相萃取-高效液相色谱法对黄曲霉毒素B1、B2的检出限分别为0.17和0.05μg/L。将本方法应用于植物油实际样品的检测中,加标回收率在81.4%~105.3%之间,相对标准偏差为1.3%~8.6%。     

A New Near-Infrared Neutral pH Fluorescent Probe for Monitoring Minor pH Changes and its Application in Imaging of HepG2 Cells

A new near-neutral pH near-infrared (NIR) fluorescent probe utilizing a fluorophore–receptor molecular framework that can modulate the fluorescence emission intensity through a fast photoinduced electron transfer process was developed. Our strategy was to choose tricarbocyanine (Cy), a NIR fluorescent dye with high extinction coefficients, as a fluorophore, and N-methylpiperazine (MP) as a receptor. The pH titration indicated that MP-Cy can monitor the minor physiological pH fluctuations with a pKa of ～7.10 near physiological pH, which is valuable for intracellular pH researches. The probe responds linearly and rapidly to minor pH fluctuations within the range of 3.05–7.10 and exhibits strong dependence on pH changes. As expected, the real-time imaging of cellular pH and the detection of pH in situ was achieved successfully in living HepG2 cells by this probe. It is shown that the probe effectively avoids the influence of autofluorescence and native cellular species in biological systems and meanwhile exhibits high sensitivity, good photostability, and excellent cell membrane permeability.     

Validation of a Reference Gene (BdFIM) for Quantifying Transgene Copy Numbers in Brachypodium distachyon by Real-Time PCR

Brachypodium distachyon has been proposed as a new model system for gramineous plants with a sequenced genome and an efficient transformation system. Many transgenic B. distachyon plants have been generated in recent years. To develop a reliable fast method for detecting transgenic B. distachyon and quantifying its transgene copy numbers, a species-specific reference gene is of great priority to be validated both in qualitative PCR and quantitative real-time PCR detection. In this study, we first proved that the BdFIM (B. distachyon fimbrin-like protein) gene is a suitable reference gene in qualitative PCR and quantitative real-time PCR for B. distachyon. Fourteen different B. distachyon varieties were tested by both qualitative and quantitative PCRs, and identical amplification products of BdFIM were obtained with all of them, while no amplification products were observed with samples from 14 other plant species, suggesting that BdFIM gene was specific to B. distachyon. The results of Southern blot analysis revealed that the BdFIM gene was low copy number in seven tested B. distachyon varieties. In conclusion, the BdFIM gene can be used as a reference gene, since it had species specificity, low heterogeneity, and low copy number among the tested B. distachyon varieties. Furthermore, the copy number of inserted sequences from transgenic B. distachyon obtained by real-time PCR methods and Southern blot confirmed that the BdFIM gene was an applicable reference gene in B. distachyon.     

豆芽中甲硝唑、多菌灵、赤霉素、6-苄基腺嘌呤、2,4-二氯苯氧乙酸的定量检测

本文建立了快速筛查豆芽中常见添加物甲硝唑、多菌灵、赤霉素、6-苄基腺嘌呤和2,4-二氯苯氧乙酸的液相色谱定量方法。回收率为79%～96.6%,定量限在20～200μg/kg。对市场随机抽查64份豆芽样品检测发现,高达32份样品中含有1种以上添加物,主要是多菌灵、6-苄基腺嘌呤和2,4-二氯苯氧乙酸。     

胡麻籽油咪唑啉缓蚀剂的制备及其对A30钢的缓蚀效果

以胡麻籽油、羟乙基乙二胺为原料合成咪唑啉中间体,用苄基氯进行改性,得到阳离子咪唑啉衍生物。利用FT IR对合成产物进行了表征,用静态失重法、电化学极化曲线和FESEM对其缓蚀性能进行了评价,并考察了不同缓蚀剂浓度、腐蚀浸泡时间对缓蚀效果的影响,探讨了其在A30钢表面的吸附行为。结果表明,合成的缓蚀剂在盐酸体系中对A30钢有较好的缓蚀性能,在浓度为100mg/L时对低碳钢的缓蚀效率可达87%,并且其产物为阳离子型缓蚀剂,吸附满足Langmuir等温吸附方程。最后采用量子化学方法对其缓蚀剂的缓蚀机理进行了分析。     

Thermal conductivity behavior of SiC–Nylon 6,6 and hBN–Nylon 6,6 composites

A study was performed to determine the effect of the content and orientation of fillers on the thermal conductivity of a polymeric composite packed with hexagonal boron nitride (hBN) and silicon carbide (SiC) fillers. The thermal conductivity behavior of SiC–Nylon 6,6 and hBN–Nylon 6,6 composites was more dependent on the orientation and shape of the filler than on its thermal conductivity. The thermal conductivity of SiC–Nylon 6,6 composites with 59 % (v/v) isotropic SiC fillers increased from 0.25 to 3.83 W/m K. That of hBN–Nylon 6,6 composites with 62 % (v/v) anisotropic hBN fillers increased from 0.25 to 2.16 W/m K in the perpendicular direction whereas in the parallel direction it increased rapidly to 8.55 W/m K .