非洛地平缓释片释放度检测方法的比较

制备了非洛地平缓释片,对其释放度的检测方法进行考察。采用紫外分光光度法和高效液相色谱法分别测定非洛地平缓释片在1%吐温-80释放介质中的释放度,并分别对两种方法进行了方法学验证。结果表明紫外分光光度法和高效液相色谱法两者都符合释放度测定的要求,且两种方法测定的释放度结果没有显著的差异。     

双氰胺高效液相色谱检测方法的研究进展

介绍了目前国内外对双氰胺的一些检测方法,包括凯氏定氮法、水解法、红外光谱法、薄层色谱法、分光光度法和高效液相色谱法,并对这些方法的优缺点进行了比较,采用高效液相色谱法更为方便和有效.综述了双氰胺运用高效液相色谱检测方法的研究进展,为双氰胺的检测提供参考和帮助.     

紫外分光光度法测定甲磺酸帕珠沙星原料药含量

采用紫外分光光度法测定了甲磺酸帕珠沙星原料药的含量,并与高效液相色谱法和酸碱滴定法的测定结果进行了比较.该法简便、快速、结果准确.为甲磺酸帕珠沙星在生产过程中的质量控制提供了可靠依据.     

pH指示剂吸光度比法测定喷昔洛韦钠原料药含量

本文采用pH指示剂吸光度比法测定喷昔洛韦钠原料药的含量,并与紫外分光光度法和高效液相色谱法两种方法进行了比较。该法简单、准确、快速、灵敏且重现性好,有应用前景。     

灰毛大青黄酮苷的分析方法和提取工艺

采用紫外分光光度法、硝酸铝-亚硝酸钠法和高效液相色谱法分别测定了灰毛大青黄酮苷含量,通过正交试验研究了灰毛大青黄酮苷提取工艺.试验结果表明3种分析方法结果相差较大,通过测定机理分析,确立了硝酸铝-亚硝酸钠法为灰毛大青黄酮苷含量测定的适宜方法,3种方法都具有较好的线性关系,精密度、稳定性、重现性和回收率均符合要求;正交试验的适宜工艺条件为料液比1∶6 （g/V）、提取温度70℃、提取时间60min和提取次数3次,在此条件下黄酮苷得率为9.9330mg/g.     

卡尔曼滤波分光光度法同时测定扑热息痛四组分的研究

卡尔曼滤波分光光度法用于测定扑热息痛合成过程中对乙酰氨基酚、对硝基酚、对氨基酚和醋酸四组分含量的研究,并详细讨论了卡尔曼滤波参数的选择。试验表明,用均匀设计法配制9组混合标准液,用多元线性回归法求出四个组分在各波长点上的吸收系数矩阵,在206-320 nm内滤波58次,便能不经分离同时测定样品中的四个组分。各组分的标准加入回收率在97.3％-109.3％之间。样品的测定结果与高效液相色谱法相符。     

分光光度法测定日化品中的三氯生

建立了分光光度法测定日化品中三氯生的方法。在酸性条件下,亚硝酸钠和对氨基苯磺酸生成重氮盐,三氯生在碱性条件下与此重氮盐发生偶合反应,形成的黄色偶氮化合物,其在452nm处有最大吸收。三氯生浓度在0.075—30mg/L范围内呈良好的线性关系,检出限为0.075mg/L。本方法成功应用于日化产品中三氯生的测定,与高效液相色谱法相比,结果令人满意。     

高效液相色谱法和硫氰酸钾滴定法检测煤中氯的比较研究

比较了测定煤中氯的高效液相色谱(HPLC)法和硫氰酸钾滴定法。以密闭氧弹燃烧或艾氏卡剂熔融分解样品，分别以高效液相色谱法和硫氰酸钾滴定法测定煤中氯，通过对国家标准物质GBW11118、GBW11119、GBW11120分析结果的比较及t检验，表明两方法无显著性差异。     

红外分光光度法测定水体中石油类及萃取剂的选择

与重量法、紫外分光光度法、荧光分光光度法和非分散红外法相比,红外分光光度法具有灵敏度高、适用范围广和测定结果受标准油品及样品中油品组成影响较小的优点。在萃取剂的选择上,建议采用六氯四氟丁烷(S-316),它具有毒性小,萃取率高,准确度和精密度好等特点,完全可用作测定水与废水中石油类的提取剂。     

杂多酸(蓝)分光光度法在测定痕量元素中的研究进展

杂多酸能被还原为有颜色的杂多蓝,结合分光光度法,可对痕量元素进行准确的分析。目前,杂多酸分光光度法作为一种分析技术,具有精度高、操作简便、分析速度快等优点,在痕量分析领域得到了迅速发展。文章综述了杂多酸在测定痕量元素P, As, Si和V中的应用及研究进展。方法主要包括钼蓝法、杂多酸-碱性染料法、荧光分光光度法、流动注射分光光度法、原子吸收分光光度法、激光热透镜分光光度法等,并对这些方法进行了比较分析。     

Molecular properties of selenomaltols: new interesting ligands for bioactive metal complexes

Properties of numerous selenium derivatives of maltol (3‐hydroxy‐2‐methyl‐4H‐pyran‐4‐one), which is an important ligand in medicinal chemistry, were studied. Selenium derivatives were obtained using consecutive in silico replacements of maltol oxygen atoms, which produced three mono‐substituted, three di‐substituted and one tri‐substituted derivatives. The geometry optimisations for these compounds in neutral, anionic and cationic forms were performed at the B1LYP/6‐311++G** level of theory. The aromatic properties of the considered selenium compounds were studied in their heterocyclic rings using several indices of aromaticity: harmonic oscillator model of aromaticity, nucleus independent chemical shift(0), nucleus independent chemical shift(1), aromatic stabilisation energy, H index, para delocalisation index and multicentre index. The methods cover all of the main types of aromaticity indices: geometric, magnetic, energetic and electronic. The calculated data show the identical aromaticity order (cation > neutral molecule > anion) for maltol and its thio and seleno derivatives. The predicted aromaticity levels of selenomaltols were compared with the previously studied maltol and various thiomaltols. Copyright © 2015 John Wiley & Sons, Ltd.     

Influence of substitution of oxygen by sulfur on maltol properties

Replacing oxygen by sulfur in a maltol molecule generates a family of new very interesting ligands: thiohydroxypyrones. In this work, theoretical calculations have been performed for all possible maltol derivatives created by consecutive substitutions of oxygen atoms by sulfur. The study is focused on molecular properties of thioligands, which are important for the formation of their metal complexes and potentially useful in medicinal and environmental chemistry. Energetic, tautomeric, aromatic, and charge distribution data are reported and the results are compared with maltol properties. It is shown that, similar to maltol, the most stable tautomer for all thio derivatives, is the one with the keto‐enol group. The protonation in cations occurs always on the heteroatom of the (thio)ketone group. The study has been carried out with the aid of some aromaticity indices, such as HOMA, NICS, and ASE. Aromaticity is studied in the heterocyclic pyran ring and in the XCCX part (where X – oxygen or sulfur). All calculations were performed at the B1LYP/6‐311++G(d,p) level of theory. We conclude that the aromaticity order determined previously for maltol (cation > neutral molecule > anion) is also preserved for thiohydroxopyrones. The results of the population analysis indicate that upon protonation, a large portion of additional positive charge delocalizes on the entire molecule, whereas upon deprotonation, negative charge accumulates mainly on the heteroatoms of the XCCX group. Copyright © 2009 John Wiley & Sons, Ltd.     

GC-MS测定仲丁醇、富马酸二甲酯、咪唑和芝麻酚

建立了气相色谱串联质谱（GC-MS）准确、快速测定香精香料中仲丁醇、富马酸二甲酯、咪唑和芝麻酚的分析方法.样品经甲醇超声提取15min后,通过Agilent DB-WAX（0.25mm×30m×0.25μm）色谱柱分离,质谱进行定性,外标法对于4种目标物质进行定量分析.实验结果表明,在0.5-20mg/L的范围内,4种物质具有较好的线性,各待测物质的线性相关系数均大于0.9990,检出限为0.02-0.12mg/L,在1,5mg/L和10mg/L 3个加标水平条件下,4种禁限用物质的平均回收率为88.0％-113.1％,相对标准偏差为0.32％-6.53％.该方法前处理简单,灵敏度高,线性相关性好,重复性佳,可以满足香精香料中4种物质的同时检测.     

主成分回归法建立卷烟风格与组分的定量关系

为研究卷烟风格与卷烟化学成分之间的关系,应用主成分回归建立卷烟GC-MS数据与卷烟风格评吸值之间的定量模型.对于每种卷烟风格,均建立了4种候选模型,然后选取最佳者.通过最佳模型对测试集样品的30种风格进行预测,有23种风格的预测值与评吸值之间的平均绝对误差小于专家评吸时的最小计分单位,所以定量模型的预测结果可靠.此研究表明化学计量学方法在处理卷烟这种复杂体系时的可用性和有效性.这些定量模型可以作为专家评吸卷烟风格的辅助工具.在定量关系不明确的情况下,应当建立多个候选模型,然后从中选择最佳者.     

ICP-MS等三种测定蛹虫草硒含量方法的比较

采用微波消解法对试验样本进行消解,分别通过ICP-MS法、HPLC/荧光法和3,3-二氨基联苯胺比色法三种方法测定了富硒蛹虫草菌丝体中硒的含量,对上述几种硒含量测定方法的工作条件、检出限和精确度进行了对比研究.实验结果表明:ICP-Ms法、HPLC/荧光法和3,3-二氨基联苯胺比色法的检出限分别为0.260 7,0.182 1和10.485 9μg·L-1,ICP-MS法的检出限最低,3,3-二氨基联苯胺比色法的检出限最高.在精密度方面.对同一样品以ICP-MS法测硒的标准差为最低,以3,3-二氨基联苯胺比色法测硒为最高.建议当分析样品中硒含量很低时,可选用HPLC/荧光法和ICP-MS法,如分析样品含硒量相对较大,可采用3,3-二氨基联苯胺比色法.     

Adamantyl pyran-4-one derivatives and their in vitro antiproliferative activity

Molecular Diversity - Pyran-4-one (maltol, kojic acid and chlorokojic acid 1) esters of adamantan-1-ylacetic acid were prepared through efficient synthetic routes in good yields and evaluated for...     

One flavor mass reweighting in lattice QCD

One flavor mass reweighting can be used in lattice QCD computations to fine tune the quark masses to their physical values. We present a new method that utilizes an unbiased stochastic estimation of the one flavor determinant. The stochastic estimation is based on the integral representation of the determinant of a complex matrix, which we prove. In contrast to other methods it can also be applied in situations where the determinant has a complex phase. The stochastic error is controlled by determinant factorizations based on mass interpolation and Schur decomposition. As an example of an application we demonstrate how the method can be used to tune the up–down quark mass difference.     

Flavor and LHC searches for new physics

Uncovering the physics of electroweak symmetry breaking (EWSB) is the raison-d’etre of the LHC. Flavor questions, it would seem, are of minor relevance for this quest, apart from their role in constraining the possible structure of EWSB physics. In this short review article, we outline, using flavor-dependent slepton physics as an example, how flavor can affect both searches for supersymmetry, and future measurements aimed at understanding the nature of any new discoveries. If the production cross-sections for supersymmetry are relatively low, as indicated by the fact that it has not revealed itself yet in standard searches, the usual assumptions about the superpartner spectra need rethinking. Furthermore, one must consider more intricate searches, such as lepton-based searches, which could be susceptible to flavor effects. We start by reviewing the flavor structure of existing frameworks for mediating supersymmetry breaking, emphasizing flavor-dependent models proposed recently. We use the kinematic endpoints of invariant mass distributions to demonstrate how flavor dependence can impact both searches for supersymmetry and the Inverse Problem. We also discuss methods for measuring small-mass splittings and mixings at the LHC, both in models with a neutralino LSP and in models with a charged slepton (N)LSP.     

胡椒生物碱提取、几何结构以及红外光谱的研究

以海南胡椒果为原料,95%乙醇溶液为溶剂,采用回流法提取胡椒生物碱。通过调节pH值除去胡椒酸,乙醚除去脂溶物,用丙酮为溶剂重结晶纯化胡椒生物碱,并用高效液相色谱仪检测其纯度,以及对胡椒生物碱进行了红外光谱表征。同时运用密度泛函B3LYP/6-31G(d, p)方法,对胡椒生物碱的结构进行优化、频率和能量的计算,得到四种构型(构型Ⅰ胡椒碱、构型Ⅱ异胡椒碱、构型Ⅲ异胡椒脂碱和构型Ⅳ胡椒脂碱)的64种构象的稳定结构,并利用吉布斯自由能计算常温(298.15 K)下四种构型分子体系稳定构象的热力学平衡分布。并对实验红外光谱与理论红外光谱的特征峰进行了对比。结果表明,所提取的胡椒生物碱主要以构型Ⅰ中的构象1结构存在,即胡椒碱结构;经纯化后得到胡椒碱含量为7%,纯度达99%。经分析建立的胡椒生物碱提取、分离和纯化方法效果良好,建立的胡椒生物碱模型能与实验结果相吻合。该研究对指导胡椒生物碱的提取、结构模型的建立、表征和应用有重大意义。