Quantification of Structurally Alert Mutagenic Impurities in Meropenem Trihydrate Drug Substance by Liquid Chromatography with High Resolution Mass Spectrometer (LC-HRMS)

Potential mutagenic impurities in Active Pharmaceutical Ingredient, Meropenem Trihydrate were assessed and a novel analytical method for their quantification was developed and validated. This Liquid Chromatographic method using High Resolution Mass Spectrometer (LC-HRMS) technique is proved to be suitable for simultaneous quantification of all ten identified impurities with required specificity, sensitivity, resolution, precision, accuracy, and other method characteristics as per ICH Guidelines. The acceptable limit of less than 2.9 μg/g was considered for evaluations, based on drug substance dosage and duration of treatment. The method stands most sensitive with a Limit of Detection of 0.35 μg/g, considering the challenge full acceptance criteria as per current regulatory standards.

晶体zinc 1-malate trihydrate∶Cu^(2+)的自旋哈密顿参量及局部结构的理论研究

在晶体场理论的基础上,利用四角对称3d9离子自旋哈密顿参量高阶微扰公式计算了Zinc 1-malate trihydrate:Cu2+的g因子(g//,g⊥)和超精细结构常数(A//,A⊥)。结果表明,由于Jahn-Teller效应,Zinc 1-malate trihydrate:Cu2+晶体中配体氧八面体沿C4轴方向伸长约0.0033 nm,络离子[CuO6]10-的键长R//≈0.2157 nm,R⊥≈0.2058 nm;局域结构沿C4轴方向呈伸长八面体结构。所得EPR参量理论计算与实验符合较好,并对上述结果进行了讨论。

Variation of soda content in fine alumina trihydrate by seeded precipitation

High soda content in fine alumina trihydrate（ATH） limits its application and increases the soda consumption. The variation of soda content in the fine ATH by seeded precipitation was determined by detection of electric conductivity of solution, soda content in ATH, measurement of particle size distribution and microscopic analysis. The results show that high concentration of sodium aluminate solution, ground circulative seed, low temperature or fast initial precipitation rate increases the soda content in ATH. Soda mainly exists in lattice soda and less soda in desilication product （DSP） exists in the fine ATH precipitated from sodium aluminate solution with concentration of Al2O3 （ρAl2O3） more than 160 g/L and mass ratio of alumina to silica （μSiO2） of 400, and lattice soda decreases with increasing initial precipitation temperature, aging seed, and low precipitation rate and precipitation time. Results also imply that -＋ 4）Na Al（OH ion-pair influences lattice soda content in ATH on the basis of electric conductivity variation.

Surface properties of superfine alumina trihydrate after surface modification with stearic acid

The surface properties of superfine alumina trihydrate （ATH） after surface modification were studied by measuring the contact angle, active ratio, oil adsorption, total organic carbon, adsorption ratio, and Fourier transform infrared （FTIR） spectrum. The contact angle increased initially and then slowly decreased with an increase of the amount of stearic acid. However, the surface flee energy decreased ini- tially and then increased. Surface modification with stearic acid or sodium stearate can benefit from elevating temperature. The base surface tension component and the free energy of Lewis acid-base both declined sharply following the surface modification. Excess stearic acid was physically adsorbed in the form of multilayer adsorption, and an interaction between oxygen on the ATH surface and hydroxyl in stearic acid was subsequently determined. Our results further indicated that the contact angle and adsorption ratio can be used as control indicators for surface modification compared with active ratio, oil adsorption and total organic carbon.

Measurement and correlation of solubility of meropenem trihydrate in binary(water＋acetone/tetrahydrofuran) solvent mixtures

The solubility of meropenem trihydrate in water+acetone mixtures and water+tetrahydrofuran mixtures were determined from T=(278.15 to 303.15) K by static method under atmospheric pressure.Effects of solvent composition and temperature on solubility of meropenem trihydrate were discussed.To extend the applicability of the solubility data,experimental solubility data in two kinds of binary solvent mixtures were correlated by the Apelblat equation and NIBS/Redlich–Kister model.It was found that the two models could satisfactorily correlate the experimental data and the Apelblat equation could give better correlation results.

Interaction of cetyltrimethylammonium bromide with cefixime trihydrate drug at different temperatures and compositions: Effect of different electrolytes

Herein,conductivity measurements have been carried out to explore the interaction between cetyltrimethylammonium bromide(CTAB,a cationic surfactant) and antibiotic drug(cefixime trihydrate(CMT)) in water and also in occurrence of inorganic salts(NaCl,Na2 SO4 and Na3 PO4) over the temperature range of 303.15-323.15 K with an interval of 5 K.In all cases,two critical micelle concentrations(c^*) were achieved for the CMT-surfactant system.Addition of CMT drug to CTAB solution decreases the values of c^* which indicates the interaction between CMT and CTAB.Both values of c^* for CMT-CTAB mixture in the presence of salts are lower in magnitude compared to the aqueous medium which indicates that micellization of the CMT-CTAB mixed system is favorable in salt solution.The values of △Gm^0 were obtained to be negative indicating the spontaneity of the micellization process and the extent of spontaneity further increases by means of rising temperature.The obtained outcomes from the ΔHm^0 and ΔSm^0 values disclose that the interactions between CMT and CTAB are mostly electrostatic along with hydrophobic in nature.The thermodynamic parameters of transfer and enthalpy-entropy compensation phenomenon were also determined and discussed in detail.

Effect of concentration of ATH on mechanical properties of polypropylene/aluminium trihydrate(PP/ATH) composite

Aluminium trihydrate(ATH) is being extensively added to polypropylene(PP) to make a fire retardant composite. Blends of PP/ATH composite are more fire resistant as compared to pure PP. Percentage proportion of both the constituents in the final composite depends upon the application. Improvement in the fire retardant properties of such composites have been studied and published in literature but effects on mechanical strength have not been addressed. The effect of concentration of ATH on the strength of PP/ATH composite was presented. The tensile, flexural and fracture properties were studied and discussed. Experimental tests, ASTM analytical formulae and finite element approach were used. It has been found that increase in ATH has an inverse effect on the mechanical strength.

Optimization and Characterization of Nano Aluminum Trihydrate-Based Flame-Retardant Materials in the Rotating Packed Bed Reactor

A CO2/NaAlO2/H2O absorption-reaction system was adopted to prepare nano aluminum trihydrate (ATH) particles for cables use in a rotating packed-bed (RPB) reactor (Phase I). The Taguchi experimental design was used to give an orthogonal array, L9(34). The parameters were the speed of rotation (A), gas-liquid flow rate ratio (B), aging temperature (C) and aging time (D), each having three levels. According to the signal/noise (S/N) ratio analysis, optimum condition for BET area (Sw) was found to be A3B3C1D1, while the parameter significance was DABC. Empirical formula for Sw was also obtained and discussed. Subsequently, the optimum size (10.7 nm) of ATH powders was used to blend with the matrix including plastics and additives (Phase II) for characterization further. The examination of composite materials showed that the limiting oxygen index (LOI) was higher than 28, indicating an excellent fire-retarding property. The results also showed that the LOI for nano ATH is higher than that bought from the market, while the fire-retarding grade examination (UL-94 test) for both ATHs was found to be of a V-0 grade. In addition, the mechanical properties for nano ATH were measured prior to using the ATH from the market.

Improvement of the Subcooling Problem of Sodium Acetate Trihydrate by a Combination of Stirring or Internal Electric Field and Nucleating Agent

Energy storage devices are the hub of a multi-energy complementary distributed energy system.Hydrated salts are the most suitable phase change material for energy storage devices,but subcooling is the main obstacle to their application.Nucleation requires a driving force so the use of nucleating agents alone does not reduce subcooling to a very low level.To address this issue,this paper first screened nucleating agents and then further reduced the subcooling of sodium acetate trihydrate in conjunction with stirring or direct current.The effects of rotor mass,rotational speed,direct current voltage,and electrode material on nucleation were analyzed.Finally,the stability of the composite phase change material in the presence of simultaneous stirring and energization was analyzed.The results showed that the addition of 1.5%in weight of disodium hydrogen phosphate dodecahydrate to sodium acetate trihydrate can reduce the subcooling to about 2.3℃.Continued addition of stirring or electricity can reduce the subcooling of sodium acetate trihydrate to within 0.5℃ or even eliminate it.The higher the momentum of the stirring,the better the improvement in subcooling,phase separation,and thermal conductivity.The higher the direct current voltage,the better the nucleation effect,but the electrode life will be lower.The silver electrode has the best nucleation effect.No new material was produced in the solution after 100 cycles in the presence of both stirring and direct current.The melting point of the phase change material was increased by 0.2℃ and the latent heat value decreased by 1.8%,still with good stability.The trace of deionized water should be added to the phase change material in subsequent studies to compensate for the consumption ofwaterby theanodicelution.

Thermal Property Enhancement of a Novel Shape-Stabilized Sodium Acetate Trihydrate-Acetamide/Expanded Graphite-Based Composite Phase Change Material

Phase change materials(PCMs)are a kind of highly efficient thermal storage materials which have a bright application prospect in many fields such as energy conservation in buildings,waste heat recovery,battery thermal management and so on.Especially inorganic hydrated salt PCMs have received increasing attention from researchers due to their advantages of being inexpensive and non-flammable.However,inorganic hydrated salt PCMs are still limited by the aspects of inappropriate phase change temperature,liquid phase leakage,large supercooling and severe phase separation in the application process.In this work,sodium acetate trihydrate was selected as the basic inorganic PCM,and a novel shape-stabilized composite phase change material(CPCM)with good thermal properties was prepared by adding various functional additives.At first,the sodium acetate trihydrate-acetamide binary mixture was prepared and the melting point was adjusted using acetamide.Then the binary mixture was incorporated into expanded graphite to synthesize a novel shape-stabilized CPCM.The thermophysical properties of the resultant shape-stabilized CPCM were systematically investigated.The microscopic morphology and chemical structure of the obtained shape-stabilized CPCM were characterized and analyzed.The experiment results pointed out that acetamide could effectively lower the melting point of sodium acetate trihydrate.The obtained shape-stabilized CPCM modified with additional 18%(mass fraction)acetamide and 12%(mass fraction)expanded graphite exhibited good shape stability and thermophysical characteristics:a low supercooling degree of 1.75℃and an appropriate melting temperature of 40.77℃were obtained;the latent heat of 151.64 kJ/kg and thermal conductivity of 1.411 W/(m·K)were also satisfactory.Moreover,after 50accelerated melting-freezing cycles,the obtained shape-stabilized CPCM represented good thermal reliability.

高铁低硫型铝土矿的工艺矿物学研究

铝土矿主要由铝的氢氧化物、氧化物和硅酸盐矿物组成,是生产金属铝的主要原料。以某高铁低硫型铝土矿为研究对象,采用元素分析、X射线衍射和扫描电镜等方法,研究铝土矿的化学组成、主要矿物的嵌布关系、矿物表面形貌等。结果表明,矿石中Al_(2)O_(3)含量为44.22%,SiO_(2)含量为5.71%,二者的比值约为7.74。矿石中主要矿物为三水铝石,褐铁矿(水针铁矿)和勃姆石含量较少。它既含有少量石英、高岭石、绿泥石和钛铁矿,又含有微量钠长石、方解石、磷灰石、一水硬铝石、铁素体和金红石等。褐铁矿中分散有微量铝,大多数褐铁矿和石英以极细粒夹杂物的形式包裹在铝矿物集合体中。矿物粒度分析表明,铝矿物集合体嵌布粒度不小于0.074 mm的累计含量为92.50%,较集中于0.015~0.060 mm,嵌布粒度小于0.010 mm的含量为0.5%;铁矿物集合体嵌布粒度不小于0.074 mm的累计含量为34.45%,嵌布粒度小于0.010 mm的含量较高,为43.44%;石英嵌布粒度不小于0.074 mm的累计含量为40.15%,嵌布粒度小于0.010 mm的含量较高,为39.86%。矿石中的大部分铝以独立矿物的形式存在。

Effects of Nano-Aluminium on The Combustion of A PolyNIMMO-Based Propellant

Propellants containing micro-aluminium particles have been shown to produce faster burn rates than conventional gun propellants.However,they are also more abrasive than conventional propellants.Nano-material propellants have been reported to give similar benefits to micron-material propellants but without the disadvantage of increased abrasion.Tests were conducted to compare the burn rates,ignitability and wear rates of a propellant loaded with 0% aluminium,15% micro-aluminium and 15%nano-aluminium.Closed vessel tests showed a burn rate increase of 39% in the range 30-250 MPa,and 70% at low pressure(50-100MPa)for the nano-aluminium propellant compared with the baseline propellant.The micro-aluminium propellant showed only a 10%increase in the burn rate compared with the standard propellant.The ignition delay for the nano-aluminium propellant was slightly shorter than that of the baseline propellant.Substantially increased wear rates were measured for the micro-aluminium propellant.The nano-aluminium propellant showed reduced wear rates compared with the micro-aluminium propellant but these were still substantially greater than those for the baseline propellant.

碳排放CO_(2)温室效应机制

基于两个化学反应①CO_(2)+H_(2)O→H_(2)CO_(3)和②H_(2)CO_(3)+3H_(2)O→H_(2)CO_(3)·3H_(2)O,采用量子化学方法,优化获得反应物和产物分子结构,计算其红外振动光谱和化学反应的热力学数据,确定这些化合物对红外辐射的吸收与强度.研究发现,反应①和②能自发发生反应,产生H_(2)CO_(3)和H_(2)CO_(3)·3H_(2)O(三水碳酸);H_(2)CO_(3)具有较强的红外辐射吸收(重要的吸收频率1919.9 cm^(−1)和强度426.7 km/mol等),H_(2)CO_(3)·3H_(2)O具有很强的红外辐射吸收(重要的吸收频率3145.9 cm^(−1)和强度1124.2 km/mol等).因此,H_(2)CO_(3)和H_(2)CO_(3)·3H_(2)O可以作为主要物质广谱强吸收近红外和中红外辐射能,放出热量促使大气温度升高产生温室效应.此外,还研究通过碳酸盐的水化反应得到的离子化合物HCO_(3)^(−),CO_(3)^(2−),HCO_(3)^(−)·3H_(2)O,CO_(3)^(2−)·3H_(2)O的红外振动,结果表明这些物质也能强吸收红外辐射能转变成热能,增强温室效应.因此,研究找到了CO_(2)作为温室气体导致温室效应的直接科学证据和机制,由CO_(2)与H_(2)O反应转变成H_(2)CO_(3)和H_(2)CO_(3)·3H_(2)O,从而产生大气温室效应.根据地球体系和大气中碳循环与碳排放的重要性和敏感危害性,直接明确的科学依据和机制确证了大气云雾中CO_(2)气体能导致温室效应,增强了控制碳排放和温室效应的急迫性.

三水乙酸钠复合相变材料的制备与热性能研究

本工作以羧甲基纤维素钠作为增稠剂,并分别以十二水磷酸氢二钠、无水磷酸氢二钠、纳米Al_(2)O_(3)及经十二烷基硫酸钠改性的纳米Al_(2)O_(3)作为成核剂,以石墨作为导热增强剂,采用熔融共混法制备出一系列复合相变材料(composite phase change materials,CPCMs)。通过红外光谱仪、扫描电镜、差示扫描量热仪和温度采集系统对CPCMs的成分、形貌和热性能等进行综合分析,结果显示,在三水乙酸钠基体中添加2%羧甲基纤维素钠/3%十二水磷酸氢二钠或2%羧甲基纤维素钠/1%改性纳米Al_(2)O_(3)能有效解决SAT相分离和过冷度大的问题,DSC分析结果显示CPCMs的相变焓维持在247.98 J/g和244.64 J/g的水平。在三水乙酸钠基体中加入2%羧甲基纤维素钠/3%十二水磷酸氢二钠/1%石墨或2%羧甲基纤维素钠/3%十二水磷酸氢二钠/1%改性纳米Al_(2)O_(3)/1%石墨能在不提高过冷度的同时增强CPCMs的导热能力,对CPCMs进行了快速循环蓄放热实验,通过T-history法计算相对潜热的变化,结果发现,随着循环次数的增加,前者热衰减率不断增加,在循环次数达到40次后趋于稳定,热衰减约23%,而后者在经过50次循环后过冷度有增加的趋势。本研究有助于推动相变材料在储热领域的应用,并为高焓值和高稳定性三水乙酸钠复合相变材料的研发提供实验依据。

三水碳酸镁焙烧法制备纳米多孔中空棒状氧化镁研究

以MgCl_(2)·6H_(2)O为原料、(NH_(4))_(2)CO_(3)为沉淀剂,采用液相沉淀法制备前驱体MgCO_(3)·3H_(2)O,并焙烧前驱体制备获得具有纤维结构的氧化镁。主要探讨沉淀剂浓度、反应温度、焙烧温度和焙烧时间对产物的平均粒径和物相组成的影响,并探究其形成机理。结果表明:沉淀剂浓度为1.5 mol/L、反应温度40℃、焙烧温度600℃、焙烧时间120 min时,可获得纳米中空棒状氧化镁,其表面由片状物相互连接形成多孔结构,前驱体三水碳酸镁在高温焙烧过程中起到模板作用。

小球藻藻渣纤维素纳米纤维的制备及对染料的吸附研究

纳米纤维因其高比表面积、生物可降解等特性被广泛用作水处理材料。小球藻经生物炼制后的藻渣富含纤维素而不含木质素,通过相对简单的纯化就可以获得高品质的纤维素。研究通过均质法从小球藻油脂提取残留物中制备了纤维素纳米纤维(CNF),其平均直径为(4.1±2.3)nm,平均长度为(375±35.3)nm.此后,利用制备的CNFS进行亚甲基蓝(MB)和刚果红(CR)的吸附研究,发现CNF对MB的吸附符合伪一级动力学模型,对CR的吸附符合伪二级动力学模型;通过对不同浓度MB、CR吸附等温线分析表明CNF对MB、CR吸附符合Langmuir等温线,最大吸附能力分别达到161.25和181.36 mg/g。两种染料的初始pH值对CNF吸附具有显著影响,MB初始pH=8时CNF具有最大吸附能力;CR在pH值5~10范围内,pH越低CNF吸附能力越强。

三水软铝石氧化铝生产过程中草酸盐脱除工艺影响因素研究

我国的铝土矿资源日趋枯竭,使用富含有机物的三水软铝石生产氧化铝是大势所趋。进口的铝土矿由于矿源的影响,有机物的含量较高一般在0.2%~0.4%之间,所以,进口矿源所带来的草酸盐浓度增加尤其值得重视。草酸盐的脱除受多种因素的影响,其中主要影响因素有草酸盐的溶解度、草酸盐脱除不同的工艺方法以及草酸盐的苛化率三个方面。本文将针对这些影响因素的作用规律进行分析,以达到有效地引导工艺优化,提高草酸盐的脱除效率的目的,从而为寻求进一步的草酸盐脱除处理方法奠定基础。

改性三水醋酸钠的储能特性及温差发电研究

三水醋酸钠(sodium acetate trihydrate,SAT)是一种可用太阳能光热转换和热能储热的固液相变材料。然而其过冷度的存在导致储存的潜热无法及时释放利用。采用十二水磷酸氢二钠(disodium hydrogen phosphate dodecahydrate,DSP)作为分子成核剂,当DSP的添加量为3%时,SAT的过冷度被降低至0.4℃,对应的相变焓值和热导率分别为226.08 J/g和0.63 W/(m·K)。将高太阳能吸收率的碳纳米管(carbon nanotubes,CNTs)与SAT/DSP蓄热单元结合后得到了具有太阳能光热转换和热能储存SAT/DSP/CNTs的装置,实现了太阳能温差发电。研究为三水醋酸钠在太阳能利用方面提供了一种可行和有效的方法。

桂中三水铝矿床地质特征与成矿规律研究

桂中三水铝土矿资源丰富,初步查明资源量达6亿吨以上,是我国唯一大型的三水铝土矿集中区,以高铁、低铝为特点,属新的铝土矿工业类型。本文系统总结桂中三水铝矿床地质特征及成矿规律特征,得出三水铝矿床大部分处于泥盆-石炭系碳酸盐岩台地相上,矿体受构造几何学特征制约,赋存于溶蚀平原或准平原内的低丘、矮岭和台地之上的红土古风化壳中等。

超声波对三水醋酸钠相分离及结晶的影响

The effects of ultrasonic radiation on phase separation as well as the crystallization of sodium acetate trihydrate,a typical salt hydrate phase change material(PCM),were studied experimentally.It is shown that ultrasonic radiation may inhibit phase separation to a certain degree.The influence of ultrasonic radiation on crystallization is also found.The addition of PCM grain can inhibit supercooling effectively.The crystallization is related to the supercooling degree.Furthermore,the effects of ultrasonic radiation on inhibiting phase separation of salt hydrates are discussed based on theoretical analysis.