Integrated Solid-Phase Extraction,Ultra-High-Performance Liquid Chromatography–Quadrupole-Orbitrap High-Resolution Mass Spectrometry,and Multidimensional Data-Mining Techniques to Unravel the Metabolic Network of Dehydrocostus Lactone in Rats

Dehydrocostus lactone (DL) is among the representative ingredients of traditional Chinese medicine (TCM), with excellent anticancer, antibacterial, and anti-inflammatory activities. In this study, an advanced strategy based on ultra-high-performance liquid chromatography–quadrupole-Orbitrap high-resolution mass spectrometry (UHPLC–Q-Orbitrap HRMS) was integrated to comprehensively explore the metabolic fate of DL in rats. First, prior to data collection, all biological samples (plasma, urine, and feces) were concentrated and purified using solid-phase extraction (SPE) pre-treatment technology. Then, during data collection, in the full-scan (FS) data-dependent acquisition mode, FS-ddMS² was intelligently combined with FS-parent ion list (PIL)-dynamic exclusion (DE) means for targeted monitoring and deeper capture of more low-abundance ions of interest. After data acquisition, data-mining techniques such as high-resolution extracted ion chromatograms (HREICs), multiple mass defect filters (MMDFs), diagnostic product ions (DPIs), and neutral loss fragments (NLFs) were incorporated to extensively screen and profile all the metabolites in multiple dimensions. As a result, a total of 71 metabolites of DL (parent drug included) were positively or tentatively identified. The results suggested that DL in vivo mainly underwent hydration, hydroxylation, dihydrodiolation, sulfonation, methylation, dehydrogenation, dehydration, N-acetylcysteine conjugation, cysteine conjugation, glutathione conjugation, glycine conjugation, taurine conjugation, etc. With these inferences, we successfully mapped the “stepwise radiation” metabolic network of DL in rats, where several drug metabolism clusters (DMCs) were discovered. In conclusion, not only did we provide a refined strategy for inhibiting matrix effects and fully screening major-to-trace metabolites, but also give substantial data reference for mechanism investigation, in vivo distribution visualization, and safety evaluation of DL.     

DL—丙氨酸与醋酸铜固相配位反应的热化学研究

用自行研制的具有恒定温度环境的反应热量计,以ｍｏｌ．Ｌ＾－１ＨＣｌ溶液为量热溶剂,测得ＤＬ－丙氨酸与醋酸铜固相配位反应焓△ｒＨｍ＝５０．８５２ｋＪ．ｍｏｌ＾－１,从而计算了配合物ｔｒａｎｓ－Ｃｕ（ＤＬ－Ａｌａ）２的标准生成焓△ｆＨｍ＝－１０１５．４１９ｋＪ．ｍｏｌ＾－１。     

DL-苏氨酸的化学合成

使用化学方法制备 DL-苏氨酸 ,再拆分制备 L-苏氨酸工业化 ,以降低瓶颈氨基酸 - L -苏氨酸的价格 ,主要原料有甘氨酸、乙醛等 ,采用的路线为甘氨酸铜路线。改进了操作工艺 ,并对产品及中间体进行了初步鉴别。红外光谱中有各自的特征峰 ,产物的熔点、红外光谱与苏氨酸的文献值相符 ,证实了产物为苏氨酸。     

Electrically Conductive Poly(DL‐lactide)/Chitosan/Polypyrrole Complexes

Summary: The fabrication of novel conductive poly(DL ‐lactide)/chitosan/polypyrrole complex membranes is reported. Using poly(DL ‐lactide)/chitosan blends as matrices and polypyrrole as a conductive component, several kinds of membranes with various compositions are prepared. A percolation threshold of polypyrrole as low as 1.8 wt.‐% is achieved for some membranes by controlling the chitosan proportion between 40 and 50 wt.‐%. SEM images exhibit that the membranes with a low percolation threshold show a two‐phase structure which consists of poly(DL ‐lactide) and chitosan phases. Dielectric measurements indicate that there is limited miscibility between the poly(DL ‐lactide) and chitosan but polypyrrole is nearly immiscible with the other two components. Based on the structural characteristics of the membranes, the polypyrrole particles are suggested to be localized at the interface between two phases.

Dependence of conductivity of complex membranes on the PPy content. (○) PDLLA/PPy, (▪) PDLLA/ch(10)/PPy, (▵) PDLLA/ch(20)/PPy, (•) PDLLA/ch(30)/PPy, (□) PDLLA/ch(40)/PPy, and (▴) PDLLA/ch(50)‐PPy.     

Reversed phase planar chromatography of dansyl DL amino acids with bovine serum albumin in the mobile phase

Summary The chromatographic behavior of twelve dansyl DL amino acids, one D isomer and eleven L isomers on RP₁₈W/UV₂₅₄, RP₁₈W/F_254s, and Sil C₁₈–50 UV₂₅₄ plates developed with aqueous—organic solutions containing bovine serum albumin (BSA) as chiral complexing agent has been extensively investigated. Enantiomeric resolution is highly dependent on mobile phase pH and ionic strength, and on the concentration of both BSA and organic modifier. All the racemates have been resolved within a development time of 1 h 30 min. The selectivity factors () for the dansyl amino acids have been compared with those from planar chromatography for the corresponding DNP, DNPy, and Fmoc amino acids, and with those of the same dansyl derivatives on a column prepared from BSA bound to silica gel.     

基于字典投影学习的人脸识别算法

针对字典学习l0或l1范数的稀疏约束导致训练和测试阶段较高的复杂性,提出用于人脸识别的字典投影学习算法.该算法合成和分析字典,达到信号表示和分类.实验结果表明,与传统的DL方法相比,所提出的DPL方法大大降低了训练和测试阶段的时间复杂度;与KNN算法相比,具有较高的识别精度和较好的稳定性.     

Unexpected proline coordination in the copper chain polymer [Cu(μ‐Cl)2(μ‐DL‐proline‐κ2O:O′)]1∞

In catena‐poly[copper(II)‐di‐μ‐chlorido‐μ‐proline‐κ²O:O′], [CuCl₂(C₅H₉NO₂)]_n, two symmetry‐independent metal cations adopt distorted octahedral coordination, typical for d⁹ Jahn–Teller systems. Each chloride bridge is involved in both a short and a very long interaction with a Cu^II centre. The centrosymmetric crystal structure contains homochiral chains of opposite handedness which extend along the shortest lattice parameter (i.e. a). The O:O′‐bridging coordination mode of proline, although a common motif for such complexes in general, is remarkable for Cu^II; the vast majority of amino acid derivatives of this cation are characterized by N,O‐chelation.     

基于延时处理的对角加载信源数估计方法

为了解决在有色噪声背景下信息论准则算法估计信源数失效以及盖氏圆方法在低信噪比下性能下降的问题,提出了一种利用接收信号延时信息的协方差矩阵对角加载技术估计信源数的方法.首先构造接收信号的延时协方差矩阵,抑制色噪声的影响,然后对延时协方差矩阵做出变换处理,得到抑制噪声后的协方差矩阵特征值,最后对得到的特征值进行对角加载技术处理,利用信息论准则进行信号源数目的估计.仿真结果表明了该算法的正确性和有效性.     

Optimization of the determination of chemical oxygen demand in wastewaters

Chemical oxygen demand (COD) is one of the most relevant chemical parameters for the management of wastewater treatment facilities including the control of the quality of an effluent. The adequacy of decisions based on COD values relies on the quality of the measurements. Cost effective management of the minor sources of uncertainty can be applied to the analytical procedure without affecting measurement quality. This work presents a detailed assessment of the determination of COD values in wastewaters, according to ISO6060:1989 standard, which can support reduction of both measurement uncertainty and cost of analysis. This assessment includes the definition of the measurement traceability chain and the validation of the measurement procedure supported on sound and objective criteria. Detailed models of the measurement performance, including uncertainty, developed from the Differential Approach, were successfully validated by proficiency tests. The assumption of the measurement function linearity of the uncertainty propagation law was tested through the comparison with the numerical Kragten method. The gathered information supported the definition of strategies for measurement uncertainty or cost reduction. The developed models are available as electronic supplementary material, in an MS-Excel file, to be updated with the user's data.