高压下TiN的结构转变、弹性和热力学性质的第一性原理计算

 利用基于密度泛函的第一性原理,计算了高压下TiN的结构转变、弹性和热力学性质。计算结果表明：在压力作用下,TiN经历了从NaCl型结构到CsCl型结构的转变,转变压力为348 GPa;TiN的弹性系数随着压力的增加呈线性增加规律。此外,还给出了德拜温度和热容量这两个重要热力学量与温度和（或）压力的依赖关系。     

基于折线采样的高分辨率成像系统设计

针对现有的提高线阵电荷耦合器件(CCD)成像系统的图像空间分辨率的方法存在的不足,提出了一种新的采样模式,并设计了一种高分辨率成像系统。该系统利用两个相同的线阵CCD相机进行特定的空间排列,即使得相机1和相机2的CCD阵列都倾斜θ来进行扫描取像,并利用图像校正和像素插值等图像重建方法,得到高分辨率的图像。实验结果表明,倾斜角取60°的情况下,相对于单个线阵相机在θ=0°的正常采样模式下得到的采样图像,图像的空间分辨率提高了1倍,且保持了成像的视野不变。本系统工程上实现简单,十分经济且便于维护,仅利用现有的成像装置即可获取更高分辨率的图像。     

门控型像增强器开门时间测量

提出了采用超快激光脉冲与光纤阵列形成的光延时、跟CCD相机相结合的方法,对门控型像增强器进行了开门时间的测量,分析了该测量方法的可行性,建立了门控型像增强器开门时间的测量系统。用该测量方法对超高速光电分幅相机中的门控型像增强器开门时间进行了测量,得到了10,20,30,50 ns档开门时间的实验图片,与所加的快高压脉冲时间12.50,18.50,28.75,48.60 ns相比较,开门时间的测量精度得到了提高,该测量方法可用于超高速光电分幅相机曝光时间的标定。     

多级离心泵内叶轮出口压力脉动研究

为研究瞬态工况下离心泵叶轮出口处的压力脉动情况,为离心泵泄漏流道流动提供边界条件,建立了包含叶轮和导叶流道的离心泵模型,基于CFD方法计算得到了其在不同工况下的性能参数,利用测试数据对结果进行了验证。分析了瞬态工况下叶轮出口处压力的变化趋势,比较了不同工况对叶轮出口压力脉动的影响,发现叶轮出口压力随叶轮旋转呈周期性变化,压力脉动频率与转速及叶轮数量有关;偏工况时叶轮出口压力脉动趋势与额定工况基本一致,但脉动频率及脉动幅值有较大区别;随离心泵转速增加,叶轮出口处压力脉动的最大值和最小值均呈减小趋势,但幅值随转速增加而增加,且增幅明显。     

低温下JB-9014钝感炸药DSD参数研究

 爆轰冲击波动力学（Detonation Shock Dynamics,DSD）是目前研究爆轰波非理想传播的有效途径。利用DSD的广义几何光学模型,研究了大长径比药柱中爆轰波非理想传播现象,根据-30 ℃下直径为10～30 mm药柱的直径效应实验数据,利用遗传算法确定了低温下JB-9014钝感炸药的DSD参数。由DSD参数计算得到了JB-9014药柱中的定态波形和爆速,计算结果与实验结果符合。     

Analysis of sialic acid levels in Chinese intravenous immunoglobulins by high‐performance liquid chromatography with fluorescence detection

Intravenous immunoglobulin (IVIg) is increasingly used for the treatment of autoimmune and systemic inflammatory diseases with both licensed and off‐label indications. Recent studies indicated that IVIg‐mediated immunomodulation and anti‐inflammation are closely associated with the IgG sialylation, especially with IgG crystallizable fragment (Fc) sialylation. The sialic acid levels of the IgG molecules and Fc fragments in 12 IVIg preparations from six Chinese manufacturers were evaluated. The Fc fragments were derived from the papain digestion of IVIg, followed by affinity and size exclusion chromatography. The sialic acid levels in Fc fragments and IVIg preparations were determined by high‐performance liquid chromatography with fluorescence detection, after the sialic acid residues were released from the proteins. The results showed that the sialic acid levels in Chinese IVIg preparations ranged from 0.875 (mol/mol IgG) to 1.085 (mol/mol IgG), and the sialic acid levels in Fc fragments were from 0.321 (mol/mol Fc) to 0.361 (mol/mol Fc). Furthermore, the sialic acid levels of IVIg preparations and Fc fragments from different Chinese manufactures were significantly different. These findings will contribute to an increased understanding of Chinese IVIg preparations and the relationship between the sialic acid levels in IVIg preparations and their clinical efficacy in future clinical studies.     

Study of degradation behavior of besifloxacin,characterization of its degradation products by LC–ESI–QTOF–MS and their in silico toxicity prediction

Knowledge and understanding of the stability profile of a drug is important as it affects its safety and efficacy. In the present work, besifloxacin, a new, fourth‐generation fluoroquinolone antibiotic, was subjected to different forced‐degradation conditions as per International Conference on Harmonization (ICH) guidelines such as hydrolysis (acid, base and neutral), oxidation, thermal and photolysis. The drug degraded under acidic, basic, oxidative and photolytic conditions while it was found to be stable under dry heat and neutral hydrolytic conditions. In total, five degradation products (DPs) were formed under different conditions—DP1 and DP2 (photolysis), DP3 (oxidation), DP4 (acidic), DP3 and DP5 (basic). The chromatographic separation of besifloxacin and its degradation products was achieved on a Sunfire C₁₈ (250 mm × 4.6 mm, 5 μm) column with 0.1% aqueous formic acid–acetonitrile as a mobile phase. The gradient RP‐HPLC method was developed and validated as per ICH guidelines. The degradation products were characterized with the help of LC–ESI–QTOF mass spectrometric studies and the most likely degradation pathway of the drug was proposed. In silico toxicity assessment of the drug and its degradation products was carried out, which indicated that DP3 and DP4 carry a mutagenicity alert.     

Stable isotope dilution assay for the accurate determination of tricaine in fish samples by HPLC–MS–MS

Tricaine methanesulfonate is one of most commonly used anesthetics in fish during blood sampling, artificial propagation and long‐distance transportation. In this study, an accurate method for the quantitative determination of tricaine in fish samples by a stable isotope dilution assay coupled with high‐performance liquid chromatography–triple quadrupole mass spectrometry was developed. Tricaine‐D₅ was synthesized and used as an isotopically labeled internal standard for the determination of tricaine. The analytical performance of the method was validated for tricaine determination in marine fish and freshwater fish. The determination of tricaine was linear in the range of 2.0–200.0 μg L^?1. The limit of detection and limit of quantitation for fish muscle tissues were 1.0 and 4.0 μg kg^?1, respectively. Good recoveries were obtained in the range of 92.08–97.50%. The inter‐ and intra‐assay relative standard deviations (RSD values) were investigated, and the values were 0.39–3.01 and 0.85–2.77%, respectively. The values of CCα and CCβ were 10.21–10.43 and 10.42–10.87 μg kg^?1, respectively. The clearance of MS‐222 from grass carp was further studied using our method. The results demonstrate that MS‐222 could be well absorbed and rapidly eliminated after bath administration.     

Densitometry and indirect normal‐phase HPTLC–ESI–MS for separation and quantitation of drugs and their glucuronide metabolites from plasma

The present work describes novel methods using densitometry and indirect or off‐line high performance thin‐layer chromatography–mass spectrometry (HPTLC–MS) for the simultaneous detection and quantification of asenapine, propranolol and telmisartan and their phase II glucuronide metabolites. After chromatographic separation of the drugs and their metabolites the analytes were scraped, extracted in methanol and concentrated prior to mass spectrometric analysis. Different combinations of toluene and methanol–ethanol–n‐butanol–iso‐propanol were tested for analyte separation and the best results were obtained using toluene–methanol–ammonia (6.9:3.0:0.1, v/v/v) as the elution solvent. All of the drug–metabolite pairs were separated with a homologous retardation factor difference of ≥22. The conventional densitometric approach was also studied and the method performances were compared. Both of the approaches were validated following the International Conference on Harmonization guidelines, and applied to spiked human plasma samples. The major advantage of the TLC–MS approach is that it can provide much lower limits of detection (1.98–5.83 pg/band) and limit of quantitation (5.97–17.63 pg/band) with good precision (?3.0% coefficient of variation) compared with TLC–densitometry. The proposed indirect HPTLC–MS method is simple yet effective and has tremendous potential in the separation and quantitation of drugs and their metabolites from biological samples, especially for clinical studies.     

Effect of quality control on the proliferation of the extract from Taraxacum mongolicum Hand.‐Mazz. in Lactobacillus plantarum

In recent years, the fingerprint of high‐performance liquid chromatography has been extensively applied in the identification and quality control of traditional Chinese medicine. It can be a potential protocol for assessing the authenticity, stability and consistency of traditional Chinese medicine and guaranteeing the expected biological activity. In this paper, a method using high‐performance liquid chromatography to identify and control the quality of the extract of Taraxacum mongolicum Hand.‐Mazz. (TME) was established. With this method, the correlation coefficients of the similarity of 10 batches were ≥0.994. The TME displayed a steady proliferative effect in Lactobacillus plantarum. In brief, this study successfully built a reliable, simple and efficient method to control and confirm the quality and the stability of biological activity of the TME.