Effect of pH,phosphate buffer concentration and the ionic strength on the stability of cefotetan disodium

Abstract

The stability of cefotetan disodium between the pH range 2-8 has been studied using a stability-indicating HPLC assay method. The optimum pH range of stability appears to be 3.6-6.4. At pH 2 or 8, the decomposition was approximately 2 times faster than between pH 3.6-6.4. The HPLC method used is accurate and precise with percent relative standard deviation of 1.0 based on 5 readings. The decomposition of cefotetan followed first-order law. The K_h and K_oh values were estimated to be 3.8 and 4.4 × 10⁴ d^-1.     

Stability of Vancomycin Hydrochloride Solutions at Various PH Values as Determined by High-Performance Liquid Chromatography

A stability-indicating HPLC assay method for the quantitation of vancomycin HCl has been developed. The developed method was used to study the effect of pH, phosphate buffer concentration and ionic strength on the stability of vancomycin HCl. The pH-rate profile curve showed 3 regions, acid-catalyzed, general base-catalyzed and the pH-independent region. The region of maximum stability was between pH 3.0 to about 5.7. On increasing the buffer concentration, phosphate ions hastened the decomposition of vancomycin HCl, the effect being more pronounced at pH 6.85 than at pH 4.43. In the pH region of 1-3, the decomposition was catalyzed by H⁺ and between pH 3-7 by HPO₄^2-, H₂PO₄^- and OH^-. An increase in the ionic strength decreased the rate of decomposition.     

Fabrication and Characterization of Potassium Ion-Selective Electrode Based on Porous Silicon

Porous-silicon (PS)-based potassium ion-selective microelectrode (K⁺ISME) was fabricated by using a microelectronic planar process and an electrochemical anodization etching technique. The apparent sensing area of the K⁺ISME is 100times100 mum ². The response time t_95% is 20 and 31 s when the concentration change is from low to high and vice versa, respectively. The potentials are constant at pH 2-8. The calibration curve for the K ⁺ISME is linear within a wide range of pK=2.0~6.0. Its average slope during six months is 56.5 mV per decade, which is close to the Nernst response. The detection limit was found to be on the order of 5times10^-7 M. The potentiometric selectivity coefficients (K_i,j ^pot) of the K⁺ ISE were 1.8 for NH ₄ ⁺, 3.6 for Li⁺, 4.1 for Na⁺, 4.5 for Mg²⁺, and 4.8 for Ca²⁺, respectively. Good performances of the K⁺ISME are attributed to large specific surface area and excellent adhesion between sensing membrane and the surface of PS     

Storage Stability of Polyynes and Cyanopolyynes in Solution and the Effect of Ammonia or Hydrochloric Acid

The storage stability of an acetonitrile solution of polyynes and monocyanopolyynes was studied by liquid chromatographic analysis for about 50 days at room temperature in a closed Pyrex flask. Monocyanopolyynes decomposition starts immediately after their synthesis; the decomposition can be approximated by a pseudo-first-order kinetic law and the rate constant is dependent from the length of the monocyanopolyyne chains, being faster for longer chains. For instance, for HC₇N the decomposition rate is k=-3.4×10^-7 s^-1 but becomes -7.0×10^-5 s^-1 for HC₁₃N decay, 204 times faster than the decay of the former compound. Polyynes mixed with monocyanopolyynes in the same CH₃CN show an induction time before starting to decompose. The induction time appears linked to the decomposition of monocyanopolyynes, which seems to protect the polyynes from the decomposition. Once the monocyanopolyynes are vanished also the decomposition of polyynes starts with a slower kinetics than monocyanopolyynes and following the rule that longer chains disappear at higher speed than shorter chains. For example, the pseudo-first-order rate constant for C₈H₂ is k=-1.31×10^-8 s^-1. Ammonia exerts a deleterious effect on monocyanopolyynes. In fact, ammonia addition to an acetonitrile solution of monocyanopolyynes causes their immediate decomposition due to a nucleophilic addition of ammonia to the polyyne chains. Instead, hydrogen-teminated polyynes are much more resistant toward the nucleophilic addition of ammonia. Hydrochloric acid does not influence the stability of polyynes and monocyanopolyynes.     

Comparing HPLC and UV spectrophotometric analysis methods for determining the stability of sorbic acid in nonionic creams containing lactic acid

This paper describes a comparison between ultraviolet (UV) spectrophotometric and high-performance liquid chromatographic (HPLC) methods of analysis for the determination of sorbic acid in nonionic creams containing lactic acid. Sorbic acid is an antimycotic agent and is used as a preservative in pharmaceuticals, cosmetics, and food products. UV spectrophotometric analysis was done by calculating the concentration of remaining sorbic acid from the absorbance values and the molar extinction coefficient E²⁵⁸_M = 24,080. A decrease in absorbance at 258 nm was accompanied by a simultaneous increase in total carbonyls and monoaldehyde content and the appearance of a very weak absorption maximum between 215 and 225 nm. HPLC analysis was done with a Hypersil BDS C₈ column with detection at 254 nm and employing a mobile phase consisting of a mixture of buffer and methanol (7:3 v/v) at a pH of 2.25. The buffer consisted of 0.85% H₂SO₄ in 17.5 mM KH₂PO₄. The validation results, together with statistical treatment of the data, demonstrated the reliability of both procedures. A drawback of the UV methods was, however, its lack of adequate measurement of sorbic acid stability at higher temperatures. For these assays, the HPLC method was found to be adequate, and it should therefore be used to obtain accurate stability data for sorbic acid in creams.     

MnO2纳米棒-还原石墨烯复合修饰玻碳电极用于苋菜红的检测

利用电化学还原法制备MnO₂纳米棒-还原石墨烯复合修饰电极（MnO₂ NRs-ErGO/GCE）用于苋菜红的检测。采用SEM和XRD分别对修饰电极材料进行微观形貌和成分结构表征。通过循环伏安法考察了苋菜红在裸电极、ErGO/GCE和MnO₂ NRs-ErGO/GCE上的电化学行为,并对测定条件如pH值、富集电位、富集时间进行了优化。结果表明,MnO₂ NRs-ErGO增大了GCE电化学活性面积,提高了苋菜红的电化学氧化响应。在最优的检测条件下,MnO₂ NRs-ErGO/GCE线性扫描伏安法检测苋菜红线性范围为2.0×10^-8~1.0×10^-5 mol/L和1.0×10^-5~4.0×10^-4 mol/L,检测限为1.0×10^-8 mol/L。MnO₂ NRs-ErGO/GCE用于真实饮料样品检测,获得满意结果。     

Inclusion Complexes of Tolnaftate with β-Cyclodextrin and Hydroxypropyl β-Cyclodextrin

Tolnaftate, an antifungal agent, was found to form inclusion complexes with both β-cyclodextrin (β-CD) and hydroxypropyl β-cyclodextrins (HPBCDs) with two different degrees of substitution [HPBCD(A)-8% and HPBCD(B)-3%]. Complex formation in the solution state was studied using phase solubility and spectral shift methods. Solid complexes were prepared by the coprecipitation method. Solubilities and dissolution rates were determined for each solid complex, its corresponding physical mixture, and free drug. The increase in solubility of tolnaftate with added HPBCD was found to be significantly greater than with added β-CD. For both HPBCD(A) and HPBCD(B), over the concentration range 0-0.05 M. 1:1 complexes with stability constants of 1460 ± 139 M^-1 and 1860 ± 165 M^-1 were observed, respectively. Over the β-CD concentration range 0-0.02 M, a 1:1 complex with a stability constant of 1190 ± 105 M^-1 was observed. At higher HPBCD concentrations, the increase in solubility was observed to show a positive deviation from linearity (type A_p phase diagram). Using the spectral method, in a 2 5% v/v methanol in water system, the stability constants were determined to be 1020 ± 150 M^-1 1110 ± 120 M^-1 and 1100 ± 260 M^-1 for HPBCD(A), HPBCD(B) and β-CD, respectively. The solid complexes prepared showed improved dissolution over physical mixtures and free drug.     

针状碳酸钙制备中氯化镁晶型导向剂的套用研究

以MgCl₂为晶型导向剂制备了形貌规整的文石相针状碳酸钙, 其粒径为2.5~5.0μm, 长径比为10~20. 采用EDTA络合滴定碳化后回收滤液中Ca²⁺、Mg²⁺含量以确定需补加MgCl₂量, 并在相同的碳化工艺条件下逐步改进套用回收液的方法制备针状碳酸钙. 产品用SEM、XRD进行形貌观察和晶型组成分析. 结果表明, 随着套用次数的增加, 碳酸钙产品中文石相的含量逐渐降低, 当文石相的含量低于80%时, 针状碳酸钙的长径比也大幅下降, 同时生成大量微细立方状方解石相碳酸钙, 将不适合继续套用. 直接套用回收液时只能循环使用1次, 而将套用的回收液经补加Mg²⁺、加酸调节pH等优化处理后可使套用次数延长至12次, 这将大幅降低针状碳酸钙的生产成本.     

Gas amplification factor in neon-nitrogen filled proportional counters

The gas amplification factor in a cylindrical proportional counter filled with Ne---N₂ Penning mixtures has been measured (over the range 1 < A < 6.4 × 10³) to verify the validity of the gas gain formulae of Rose and Korff, Khristov, Williams and Sara, Diethorn and Zastawny. This factor has been found to obey Zastawny's formula over the range of variables studied. The formula of Diethorn can be fitted only for small nitrogen concentrations (below 5 × 10⁻⁴).

Constants appropriate to the Zastawny and Diethorn formulae have been determined over a wide range of N₂ concentrations from spectroscopically pure Ne up to 11.1% N₂.     

Near-Infrared Laser-Induced Decomposition of C60 Dissolved in Toluene

In this paper we describe the efficient and substantial decomposition of C₆₀ in toluene solution, induced by moderate intensity (I = 20 - 55 MW cm^-2) near infrared (γ = 1064 nm) laser radiation. This behavior is surprising since both uncharged fullerene and toluene do not have any absorption bands at this wavelength. The decomposition efficiency and products are investigated with UV-Vis absorption spectrophotometry and high-performance liquid-chromatography (HPLC). Possible mechanisms of the fullerene decomposition are discussed.     

纳米Fe3O4-还原氧化石墨烯复合修饰玻碳电极的制备及电化学检测多巴胺

通过电化学还原法制备纳米Fe₃O₄-还原氧化石墨烯复合修饰玻碳（Fe₃O₄-rGO/GCE）电极,用于多巴胺（DA）的检测。采用SEM、TEM和循环伏安对纳米Fe₃O₄-rGO复合材料进行表征。在pH为7.0的磷酸盐缓冲液（PBS）中,采用循环伏安法研究了DA在纳米Fe₃O₄-rGO/GC上的电化学行为。实验结果表明,较裸GC电极和rGO修饰（rGO/GC）电极,由于纳米Fe₃O₄与rGO的协同作用,纳米Fe₃O₄-rGO/GC显著增大了Fe₃O₄-rGO/GC复合材料电极电化学活性面积和氧化峰电流强度i_pa。DA的浓度在6.0×10^-8~2.0×10^-6 mol/L和2.0×10^-6~8.0×10^-5 mol/L范围内,与氧化峰电流强度i_pa呈良好的线性关系,检出限达4.0×10^-9 mol/L（信噪比S/N=3）。抗坏血酸和尿酸共存物几乎不干扰DA的测定,选择性高。Fe₃O₄-rGO/GC修饰电极用于盐酸DA注射液中的DA含量测定,获得结果较好,回收率为97.1%~103.9%。     

Gd2Zr2O7陶瓷的高温热物理性能及Gd2Zr2O7-8YSZ双涂层制备

通过高温固相合成方法制备了烧绿石结构Gd₂Zr₂O₇陶瓷材料,研究了其高温相稳定性和热物理性能。采用电子束物理气相沉积方法制备了Gd₂Zr₂O₇-8YSZ(8%Y₂O₃-ZrO₂)双陶瓷层结构热障涂层,分析了涂层顶层的晶体结构和原子数量比。结果表明,Gd₂Zr₂O₇在室温至1500℃范围内具有良好的相稳定性,比第一代热障涂层8YSZ的高温相稳定区间提高250℃以上。Gd₂Zr₂O₇块材的热膨胀系数在100~1500℃范围内介于8.8×10^-6~11.0×10^-6 K^-1之间,与8YSZ接近; 在1000~1400℃高温区间,热导率约为1.0 W(m·K)^-1,比8YSZ降低一半左右。沉积制得的Gd₂Zr₂O₇涂层化学成分符合化学计量比,为烧绿石结构,涂层呈现典型的柱状晶结构。     

Anaerobic stability of aqueous physostigmine solution

The anaerobic stability of physostigmine was studied in this report. Physostigmine and two important degradants, eseroline and rubreserine, were identified by a high-performance liquid chromatography (HPLC) system using a photodiode array detector and a UV detector at the retention times of 12.4, 9.2, and 7.9 min. Under anaerobic treatment, the minimum degradation rate constant was found at pH 3.4, evaluating from pH-rate profiles at 45°C, 55°C, and 70°C with the pH range 2.4-6.8. The degradation of physostigmine was suggested as specific acid-base catalysis. Anaerobic activation energies of K_H, K_OH,, and _OBS were 9.4, 8.3, and 17.9 kcal/mol, respectively. The ratios of observed aerobic and anaerobic rate constants were 2-33 at 88°C, which had a trend to increase ratios as pH increased in the range 2.4-5.2. The shelf life of physostigmine solution was estimated to be 4 years at room temperature under anaerobic conditions at pH 3.4.     

YVO4∶Eu3+,Bi3+红色荧光粉的水热合成及其荧光性能

以Y₂O₃、Eu₂O₃、Bi(NO₃)₃·H₂O、浓HNO₃、偏钒酸铵、氨水、无水乙醇和一缩二乙二醇为原料,采用聚乙烯吡咯烷酮(PVP)辅助水热法合成YVO₄: Eu³⁺, Bi³⁺纳米颗粒。使用X射线衍射(XRD)、扫描电镜(SEM)、红外光谱(IR)和荧光光谱(FL)等手段对产品进行了表征和分析。结果表明：合成的样品为YVO₄: Eu³⁺, Bi³⁺纳米颗粒,均具有四方晶相结构,其微结构随反应溶液的的pH值变化。YVO₄: Eu³⁺, Bi³⁺纳米颗粒在619 nm处有较强的红光发射(电偶极跃迁⁵D₀→⁷F₂),在594 nm有较弱的橙光发射(磁偶极跃迁⁵D₀→⁷F₁)。随着Eu/Bi比值的增大材料的荧光先增强后减弱,在Eu/Bi比值为5时样品的红光发射最强。溶液的pH值影响YVO₄: Eu³⁺, Bi³⁺纳米晶的发光强度,其中pH值为10时的样品其红光发射最强。并探讨了YVO₄: Eu³⁺, Bi³⁺纳米晶的发光机理。     

Synthesis and Characterization of Mesoporous Alumina via a Reverse Precipitation Method

Mesoporous alumina γ-Al_2O_3 with high specific surface area and large pore volume is prepared by using a facile reverse precipitation method from sodium aluminate and nitric acid.The effects of terminal pH value,aging time and thermal stability on the characterization of γ-Al_2O_3 are studied by means of X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FTIR),Brunauer-Emmett-Teller(BET) method and scanning electron microscopy(SEM).The results show that γ-Al_2O_3 with better properties can be obtained by changing the preparation parameters.High BET surface area of 340(m~2)/g can be obtained by calcining at 500 ℃ for 4 h with large pore volume of 0.90(cm)~3/g and average pore size of 7.6 nm.After calcining at 1000°,the surface area is still 86 m2/g and the pore volume is 0.37(cm)~3/g.     

Liquid-Liquid Extraction, Separation, Preconcentration, and ICP-AES Determination of Lanthanum and Cerium with N-Phenyl-(1,2-methanofullerene C60)61-formohydroxamic Acid

A novel method for liquid-liquid extraction, separation, preconcentration, and simultaneous trace determination of cerium(IV) and lanthanum(III) with N-phenyl-(1,2-methanofullerene C₆₀)61-formohydroxamic acid (PMFFA) is reported. Lanthanum and cerium are extracted at pH 8.5 and 9.5, respectively in chloroform and recovered from monazite sands in the presence of thorium, uranium, and large number of cations and anions in high purity (99.98%). The extraction mechanism is investigated. The influence of PMFFA, pH, diverse ions, and temperature on the distribution constants of lanthanum and cerium was examined. The overall stability constants (log β₂K_e) and extraction constants (K_ex) for lanthanum(III) are 22.50 and 5.0 × 10^-9, respectively and for cerium(IV) are 21.51 and 3.9 × 10^-9, respectively. Lanthanum(III) gives a colourless complex with PMFFA which is extracted into chloroform having molar absorptivity 5.5 × 10⁴ L mol^-1 cm^-1 at 395 nm, and Beer's law 0.12-2.52 µg mL^-1, while cerium(IV) forms a red coloured complex, λ_max 460 nm, molar absorptivity 1.5 × 10⁴ L mol^-1 cm^-1, and Beer's law 0.46-9.26 µg mL^-1. For trace determination the extracts were directly inserted into the plasma for inductively coupled plasma atomic emission spectrometry ICP-AES measurements of lanthanum and cerium which increases the sensitivity 60 folds and obey Beer's law in the range, 2.1-37.5 ng mL^-1 for lanthanum and 9.2-186.4 ng mL^-1 for cerium. The method is applied for the determination of lanthanum and cerium in real and standard samples, sea water, and environmental samples.     

pH对低温燃烧法合成钨酸铋光催化降解罗丹明B的影响

以低温燃烧法制备钨酸铋(LCM-Bi2WO6), 并表征了其晶体结构、形貌特征、等电点及紫外漫反射谱, 同时以染料罗丹明B(RhB)为目标污染物(25 mg/L, pH=4), 考察了所制备Bi₂WO₆的吸附性能和光催化性能, 并探讨了RhB溶液pH(1、4、7、10)及酸度调节剂成分(盐酸和硫酸)的影响。结果表明, 所制备Bi₂WO₆为正交相, 吸收极限波长为455 nm, 禁带宽度为2.72 eV, 晶格粒径为14.7 nm, 等电点为3.43; 其对RhB的吸附和光催化效果强于水热法制备Bi₂WO₆和二氧化钛(TiO₂)。不同pH溶液中, LCM-Bi₂WO₆对RhB的吸附过程和光催化过程分别符合准二级动力学方程和一级动力学方程式, 且吸附平衡量(7.48~21.93 mg/g)和光催化速率常数(0.0197~0.1181 min^-1)均随pH降低而增大。LCM-Bi₂WO₆对RhB的光催化降解主要由·OH所致。光催化过程中, RhB紫外可见光谱的蓝移现象揭示LCM-Bi2WO6可通过脱乙基-共轭显色基团断裂途径降解RhB。以H₂SO₄调节酸度时, SO₄^2-离子可被Bi₂WO₆强吸附, 从而使得LCM-Bi₂WO₆对RhB的平衡吸附量(qe为6.03 mg/g)和光催化速率(kv为0.115 min-1)远小于HCl调节(qe为21.93 mg/g, kv为0.1181 min-1)时对RhB的平衡吸附量和光催化速率。     

Low current density, inverted polarity, high-speed, top-emitting 850 nm vertical-cavity surface-emitting lasers

High-speed, oxide-confined, inverted polarity (n-up), polyimide-planarised 850 nm vertical-cavity surface-emitting lasers (VCSELs) were fabricated and characterised. The lasers exhibit a -3 dB frequency modulation bandwidth (f_3dB) up to 15.2 GHz with a 10 mum oxide aperture diameter, at the lowest current density (/bias) ever reported of 6.4 kA/cm². The ratio f_3dB ²/J_bias = 36.1 (GHz²/kA/cm²) represents a 21% increase when compared with the highest previously reported ratio. The threshold voltage and current were as low as 1.45 V and 0.9 mA, respectively, with a series resistance of 65 Omega. A rate-equation-based thermal VCSEL model was used to predict the device performance at different temperatures. Good agreements between measured and simulated DC characteristics were obtained.     

Sr2Si5N8:Eu2+荧光粉的制备及其发光性能研究

以Sr₂CO₃、Si₃N₄和Eu₂O₃为原料, 以C为主要还原剂, 采用碳热还原氮化工艺合成Sr₂Si₅N₈:Eu²⁺荧光粉, 着重研究了C、Sr₂CO₃添加量及Eu²⁺浓度对产物物相及发光性能的影响。研究结果表明: 当C与Si₃N₄的摩尔比 n_c/=9/5时,合成出Sr₂Si₅N₈:Eu²⁺单相荧光粉, 添加适当过量的Sr₂CO₃可提高合成产物的N含量, 且荧光粉的发光强度与其N含量呈现正相关关系。在450 nm蓝光激发下, 受Eu²⁺的4f⁶5d¹ → 4f⁷跃迁作用, Sr₂Si₅N₈:Eu²⁺荧光粉在550~700 nm波段范围产生非对称宽带发射。随着Eu²⁺掺杂浓度由1.5mol%增加到20mol%, 荧光粉的发光强度先增强后减弱, 达到2mol%时发生浓度淬灭现象; 发射主峰由608 nm逐步红移至641 nm; CIE色坐标从(0.606, 0.393)位移至(0.656, 0.343), 是一种可用于白光LED的优质红色荧光粉。     

Raman Spectroscopy of the Charge Transfer Complex (TTF)x C60 Br8

We report Raman studies on powder samples of the charge transfer complex (TTF)_x C₆₀Br₈ at room temperature. The phonons show considerable softening with respect to the frequencies observed in the Raman spectrum of solid C₆₀ Brg. The strongest mode at 1464 cm^-1 in C₆₀Br₈ is red shifted to a doublet with peaks at 1414 and 1421 cm^-1, implying an average phonon softening Δω of -47 cm^-1. A comparison with the phonon softening of the corresponding A_g(2) mode in alkali-doped C₆₀ (Δω ~ - 36 cm^-1 for A₆C₆₀, A = K, Rb or Cs) suggests that 8 electrons are transferred per C₆₀Br₈ molecule in the charge transfer complex. The mode at 503 cm_--1 in C₆₀Br₈ is shifted upwards, similar to that in A₆ C₆₀ compounds.