Rapid preparative isolation of erythrocentaurin from Enicostemma littorale by medium‐pressure liquid chromatography,its estimation by high‐pressure thin‐layer chromatography,and its α‐amylase inhibitory activity

Erythrocentaurin is a relatively simple natural product present among the members of Gentianaceae. A preparative method for the isolation of erythrocentaurin from the ethyl acetate fraction of Enicostemma littorale using medium‐pressure liquid chromatography has been reported. The method consisted of a simple step gradient from 10 to 20% ethyl acetate in n‐hexane. Using a 70 × 460 mm Si60 column, this method is capable of processing 20 g of material in <3 h (purity ≈ 97%). The recovery of erythrocentaurin was 87.77%. Estimation of erythrocentaurin in extracts and fractions based on high‐pressure thin‐layer chromatography was carried out on silica gel 60 F₂₅₄ plates with toluene/ethyl acetate/formic acid (80:18:2 v/v/v) as the mobile phase. The densitometric analysis was performed at 230 nm. A well‐separated compact band of erythrocentaurin appeared at R_f 0.54 ± 0.04. The analytical method showed good linearity in the concentration range of 200–1500 ng/band with a correlation coefficient of 0.99417. The limits of detection and quantification were found to be ≈60 and ≈180 ng/band, respectively. Erythrocentaurin exhibited a concentration‐dependent α‐amylase inhibition (IC₅₀ 1.67 ± 0.28 mg/mL). The outcome of the study should be considered for pharmacokinetic and biotransformation studies involving E. littorale.     

Difference Cochains and Reidemeister Traces

The authors consider the difference of Reidemeister traces and difference cochain of given two self-maps,and find out a relation involving these two invariants.As an application,an inductive formula of the Reidemeister traces for self-maps on a kind of CW-complex,including spherical manifolds is obtained.     

侵入气体沿井筒的上升规律研究

地层气体侵入井筒后形成气液两相流动体系,气体沿井筒向上滑脱运移,随着所受压力的降低其发展变化过程会很快,如果不及时处理就会演变为井涌、井喷,甚至井喷失控.因此,准确的预测侵入气体沿井筒的上升规律,有助于认识气侵发展过程,同时为现场采取井控措施提供理论依据,有效避免井下复杂事故.基于侵入气体沿井筒运动的力学特性,建立了气体的上升速度模型,模型模拟分析表明:地层渗透率越高、机械钻速越快、单位时间内侵入井筒的气体量越多、气体上升速度越快,井底压力波动越大;施加一定的井口回压可以有效抑制气体的膨胀运移.     

考虑底部隆起的浅埋隧道围岩压力计算分析

针对浅埋隧道开挖后底部隆起变形现象,应用极限分析上限法构造了考虑底部隆起变形的围岩压力计算模型,结合线性Mohr-Coulomb准则等推导出极限围岩压力的理论表达式。通过约束条件将围岩压力的计算转化为数学中的最优化问题,编制程序进行了优化计算。将计算结果与工程实测数据及文献计算结果进行了对比,验证了当前方法的可靠性。同时,指出在运用极限分析法处理浅埋隧道围岩压力问题过程中应将隧道底部一同考虑,对隧道底部支护会对整个围岩压力产生影响,有助于隧道结构的整体稳定。研究可以为浅埋隧道的开挖、支护提供一定的理论指导.     

Determination of macrolides in livestock excreta by syringe purification coupled with liquid chromatography tandem mass spectrometryEI北大核心CSCD

A method of syringe-dispersive solid-phase extraction combined with ultrahigh performance liquid chromatography with tandem mass spectrometry for the simultanous determination of 10 macrolides in manurebased fertilizers was developed. After extraction with methanol and acetonitrile,the extracts were purified by insyringe dispersion solid-phase extraction in syringes pre-filled with 60 mg PSA and 30 mg C18. The resulted extracts were further separated by a BEH C18 column,detected by multiple reaction monitoring in electrospray positive ion mode,and quantified by matrix-matched external standard method. The results showed that the recoveries of the target compounds ranged from 70% to 110% at three spiked levels（10,30,and 50 μµg/kg）with the relative standard deviations ranged from 1.4% to 12%. The limits of detection and quantification were 0.57 1.75 and 2.77-5.40 μµg/kg,respectively. This method was suitable for the simultaneous determination of residual macrolides in organic fertilizers. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

高压密闭消解-电感耦合等离子体质谱法测定青藏高原气溶胶样品中磷及其他18种元素

气溶胶中磷（P）的准确测定是评估磷沉降对青藏高原生态效应及磷的生物地球化学循环的重要前提。针对青藏高原气溶胶中磷含量低及滤膜单个样品量有限的特征,本文建立了高压密闭消解-电感耦合等离子体质谱法测定气溶胶中磷及其他元素含量的方法。电感耦合等离子体质谱法（ICP-MS）测得P元素的检出限为3.5 μg/L,优于电感耦合等离子体发射光谱仪（ICP-OES）的检测限（89 μg/L）,其他元素检出限均达到μg/L（ppb）级（0.013-36 μg/L）,部分元素如Co、Cd、Pb等达到ng/L（ppt）级（2-7 ng/L）。各元素线性关系良好,测定结果的相对标准偏差(RSD) < 5%,磷的加标回收在90-103%, 方法准确度和精密度满足分析要求。该方法成功地测定了青藏高原实际气溶胶样品中磷及其他元素,具有良好的可靠性和实用性。     

Carbon dots/Bi_2WO_6 composite with compensatory photo-electronic effect for overall water photo-splitting at normal pressure

Overall water photo-splitting is a prospective ideal pathway to produce ultra-clean H_2 energy by semiconductors.However,the band structure of many semiconductors cannot satisfy the requirement of H_2 and O_2 production at the same time.Herein,we illustrate that carbon dots(CDs)/Bi_2 WO_6 photocatalyst with compensatory photo-electronic effect has enhanced activity for overall water photo-splitting without any sacrificial agent.In this complex photocatalytic system,the photo-potential provided by CDs makes the CDs/Bi_2 WO6(C-BWO) composite could satisfy the band structure conditions for overall water photo-splitting.The C-BWO composite(3 wt% CDs content) exhibits optimized hydrogen evolution(oxygen evolution) of 0.28 μmol/h(0.12 μmol/h) with an approximate 2:1(H_2:O_2) stoichiometry at normal pressure.We further employed the in-situ transient photovoltage(TPV) technique to study the photoelectron extraction and the interface charge transfer kinetics of this composite catalyst.     

最大泡压法测表面张力等温线的数据处理方法比较*

对乙酸、丙酸、正丁酸、2-甲基丁酸、3-甲基丁酸、正戊酸、正己酸、乙醇、丙醇、异丙醇、正丁醇、异丁醇、1,2-丙二醇等13种常用试剂在25 ℃下的表面张力数据拟合方法进行了比较,分析了图解法处理数据及多项式、一阶指数函数、幂函数、Shishkovsky经验公式拟合数据的优缺点。指出Shishkovsky经验公式拟合结果准确,受数据样本量影响小,是理想的表面张力数据拟合方法。     

Kinetic study on solute permeation at the interface of molecular aggregates by partial filling capillary electrophoresis

Moment analysis method using partial filling CE was developed for the kinetic study on solute permeation at the interface of spherical molecular aggregates. Moment equations for partial filling CE were developed by classifying CE systems into five categories according to the migration velocities of solute and molecular aggregate. The method was applied to the study on the dissolution of electrically neutral solutes into SDS micelles. Elution peaks were measured by partial filling CE while changing the concentration of SDS and the filling ratio of SDS micellar zone to the capillary (ϕ_M). Partition equilibrium constants (K_p) and rate constants of interfacial solute permeation of SDS micelles (k_in and k_out) were determined from the first absolute and second central moments of the elution peaks by using the moment equations. Their values were comparable irrespective of ϕ_M and were almost the same as those previously measured by complete filling CE. The positive correlation of K_p with the hydrophobicity of the solutes was explained in terms of the change in k_in and k_out. It was demonstrated that the moment analysis method using partial filling CE is effective for studying solute permeation kinetics at the interface of spherical molecular aggregates.     

毛细管电泳法高效筛选8-氧代鸟嘌呤DNA糖基化酶的核酸适配体

8-氧代鸟嘌呤DNA糖基化酶(OGG1)是人体中重要的功能蛋白,在修复DNA氧化性损伤过程中起关键作用。氧化应激等引起的氧化损伤易导致炎症反应的发生,对OGG1的抑制可以一定程度上起到缓解作用;对癌细胞OGG1的抑制有望作为癌症治疗的新方法。目前的研究多集中于小分子对OGG1功能的影响和调控,而OGG1的适配体筛选尚未见报道。作为功能配体,适配体具有合成简单、高亲和力及高特异性等优点。该文筛选了OGG1的核酸适配体,结合毛细管电泳高效快速的优点建立了两种基于毛细管电泳-指数富集进化(CE-SELEX)技术的筛选方法:同步竞争法和多轮筛选法。同步竞争法利用单链结合蛋白(SSB)与核酸库中单链核酸的强结合能力,与目标蛋白OGG1组成竞争体系,并通过增加SSB浓度来增加竞争筛选压力,以去除与OGG1弱结合的核酸序列,一步筛选即可获得与OGG1强结合的核酸序列。多轮筛选法在相同孵育条件和电泳条件下,经3轮筛选获得OGG1的核酸适配体。比较两种筛选方法的筛选结果,筛选结果中频次最高的3条候选核酸适配体序列一致,其解离常数(K_D)值在1.71~2.64 μmol/L之间。分子对接分析结果表明候选适配体1(Apt 1)可能与OGG1中具有修复氧化性损伤功能的活性口袋结合。通过对两种筛选方法的对比,证明同步竞争法更加快速高效,对其他蛋白核酸适配体筛选方法的选择具有一定的指导意义。得到的适配体有望用于OGG1功能调控,以抑制其修复功能。