硝酸脲中酰胺态氮及总氮含量测定的研究

对硝酸脲中酰胺态氮及总氮含量进行测定。以甲醛－硫酸法分析硝酸脲中酰胺态氮时，发现酰胺态氮的含量总是与理论值相关差将近1倍。文中解释了造成这一结果的原因。并找到了导致这种结果的定量关系。从反应温度，时间等方面进行多次试验，找到了适宜的分析条件。     

含铁氢氟酸和硝酸混合酸中氢氟酸和硝酸含量的测定

在氢氟酸和硝酸的混酸中由于Fe3+的存在干扰了测定,本文讨论了对上述酸的测定方法,本法采用氟电极测定混合酸中氢氟酸的含量,其中Fe3+的干扰可加入柠檬酸三钠除去[1].用氢氧化钠作滴定剂,用玻璃电极作指示电极,用二次微商法确定滴定的体积,通过计算得出总酸的含量[2],从总酸中减去氢氟酸的含量即为硝酸的含量.     

化学计量学方法应用于近红外光谱法测定混合炸药中TNT含量

为构建样品中的被测组分(TNT)的含量与其红外光谱之间的数学模型,从生产线上采集以及按相同方法制备了共计155个样品并采集了它们的红外光谱,根据计算所得光谱残留F值判别并剔除异常光谱。随机选取63个样品的光谱作为校正集,其余92个样品的光谱作为验证集。另外采用常规的溶剂提取-红外光谱法测定了这些样品中TNT的含量作为建模参考值。在最优模型波段(cm-1)为:9 114.1～8 331.2,7 671.6～7 189.5,6 514.5～5 666,5 102.8～4 929.3,4 744.14～4 728.71的条件下,根据校正集的光谱数据,用偏最小二乘法建立数字模型。通过交叉检验均方根误差,RMSECV-维数曲线的理想程度以及光谱主成分分析结果选取了最优模型。采用χ2检验法,以及根据预测标准差和Bias值,结合验证集样品的光谱和数据,评估了方法的精确度和准确度。从TNT含量在36.68%～46.95%内的8个样品的测定结果得出其预测值的Bias值为0.078%,SEP%为0.514%。说明方法的准确度和精密度良好,且无需使用有机试剂。     

硫酸铁铵滴定法测定钨钛合金中钛的含量

建立了硫酸铁铵滴定法测定钨钛合金中钛含量的新方法。以硝酸-氢氟酸溶解样品,在25mL NaOH(100g/L)的强碱性介质中,以铁为载体,沉淀分离被测定元素钛后,用盐酸溶解沉淀。在酸性条件下,用铝片还原Ti~(4+)至Ti~(3+),以硫氰酸盐为指示剂,用硫酸铁铵标准溶液滴定至红色为终点。根据消耗硫酸铁铵滴定溶液的体积,求得样品中钛含量。按照实验方法测定样品中钛含量,结果的相对标准偏差(RSD,n=11)为0.40%,加标回收率为99.8%~101%。方法有很好的精密度和准确度,可用于钨钛合金中钛含量的分析。     

土壤易溶盐浸提液中硫酸根和硝酸根的测定

对不同地区不同深度的土壤进行前期预处理,在最佳试验条件下,应用离子色谱法测定土壤浸提液中硫酸根和硝酸根的含量,测定的相对标准偏差分别为1.9%和3.0%,加标回收率SO42-90.0%~100.0%、NO3-93.0%~101.0%.样品预处理操作简单,方法灵敏度和准确性高,结果稳定性好,检出限低,能满足土壤环境样品检验的要求.     

高效液相色谱法测定消毒湿巾中苯扎氯铵的含量

提出了高效液相色谱法测定消毒湿巾中苯扎氯铵含量的方法。样品经流动相超声提取,以Eclipse XDB-C18色谱柱(150 mm×4.6 mm,5μm)为分离柱,以乙腈-70 mmol.L-1乙酸铵(含1%三乙胺,冰乙酸调pH至5.0)按体积比70比30混合液为流动相,用二极管阵列检测器于波长262 nm处测定。苯扎氯铵的质量浓度在100～500 mg.L-1范围内与其峰面积呈线性关系,检出限(3S/N)为10.2mg.L-1。应用此法测定消毒湿巾中苯扎氯铵,回收率在95.3%～97.8%之间,相对标准偏差(n=5)在2.5%～4.0%之间。     

STUDIES OF A.C. CONDUCTIVITY OF POLY(VINYL BORATE) AND ITS CALCIUM DERIVATIVE IN SOLID STATE

An attempt has been made in the present work to prepare poly(vinyl borate),PVBO and its calcium derivative by homogeneous esterification of PVA with boric acid in non-aqueous medium in the presence of a catalyst ethyl nitrate dimethyl sulfoxide.The compounds were characterized by IR and ~1H-NMR spectra.Conductivities were determined from 30℃to 90℃in solid state within a frequency range of 42 Hz to 100 kHz.The compounds so formed showed ionic conductivity and their conductivities were dependent on frequen...     

A new triterpene saponin from Panax japonicus C. A. Meyer var major (Burk.) C. Y. Wu et K. M. Feng

<正>One new triterpene saponin was isolated from Panaxjaponicus C.A.Meyer var major(Burk.) C.Y.Wu et K.M.Feng,and established as oleanolic acid 3-O-[β-D-glucopyranosyl-(1→2)-β-D-glucuronopyranosyl-6'-O-n-butyl ester]which showed moderate antitumor activities against the A2780 cells and OVCAR-3 cells.Its structure was established by means of spectral data, particularly NMR,including HSQC and HMBC techniques.     

大孔吸附树脂分离纯化香椿叶总黄酮的研究

比较了AB-8、S-8、X-5、NKA-9、D-3520、NKA、聚酰胺、硅胶8种吸附剂对香椿叶黄酮类化合物的吸附及脱附性能.在静态吸附试验的基础上,筛选出效果较好的X-5树脂进行动态试验研究.结果表明,X-5树脂在约15℃下对香椿叶总黄酮动态吸附-脱附较优的工艺参数为:上柱液pH值5～6,上柱速度3BV/h,溶液处理量6BV/次;脱附剂为70%乙醇,脱附剂的流速3BV/h,脱附剂用量6BV/次.此工艺条件能够分离纯化香椿叶黄酮类化合物,树脂使用1次时,总黄酮的收率达95.5%,总黄酮的纯度由7.2%提高到43.5%;树脂重复使用5次时,总黄酮的收率仍达80%以上,总黄酮的纯度可由7.2%提高到20%以上.     

Quinoxalinones as A Novel Inhibitor Scaffold for EGFR (L858R/T790M/C797S) Tyrosine Kinase: Molecular Docking,Biological Evaluations,and Computational Insights

Combating acquired drug resistance of EGFR tyrosine kinase (TK) is a great challenge and an urgent necessity in the management of non-small cell lung cancers. The advanced EGFR (L858R/T790M/C797S) triple mutation has been recently reported, and there have been no specific drugs approved for this strain. Therefore, our research aimed to search for effective agents that could impede the function of EGFR (L858R/T790M/C797S) TK by the integration of in silico and in vitro approaches. Our in-house quinoxalinone-containing compounds were screened through molecular docking and their biological activity was then verified by enzyme- and cell-based assay. We found that the four quinoxalinone-containing compounds including CPD4, CPD15, CPD16, and CPD21 were promising to be novel EGFR (L858R/T790M/C797S) TK inhibitors. The IC₅₀ values measured by the enzyme-based assay were 3.04 ± 1.24 nM; 6.50 ± 3.02 nM,10.50 ± 1.10 nM; and 3.81 ± 1.80 nM, respectively, which are at a similar level to a reference drug; osimertinib (8.93 ± 3.01 nM). Besides that, they displayed cytotoxic effects on a lung cancer cell line (H1975) with IC₅₀ values in the range of 3.47 to 79.43 μM. In this proposed study, we found that all screened compounds could interact with M793 at the hinge regions and two mutated residues including M790 and S797; which may be the main reason supporting the inhibitory activity in vitro. The structural dynamics revealed that the screened compounds have sufficient non-native contacts with surrounding amino acids and could be well-buried in the binding site’s cleft. In addition, all predicted physicochemical parameters were favorable to be drug-like based on Lipinski’s rule of five, and no extreme violation of toxicity features was found. Altogether, this study proposes a novel EGFR (L858R/T790M/C797S) TK inhibitor scaffold and provides a detailed understanding of compounds’ recognition and susceptibility at the molecular level.