基于吸收系数的生脉注射液中聚山梨酯80含量测定新方法

聚山梨酯80又名吐温80，为一种亲水型非离子表面活性剂，是食品、保健品和药品中常用的辅料，作为增溶剂和澄清剂广泛用于中药注射剂。近年来，不良反应的发生使得聚山梨酯80的质量和应用愈加受到重视，有研究认为其加入可能引起注射剂不良反应增加。为避免超量使用，有必要对该辅料的投料加以严格控制。中药注射剂中聚山梨酯80的含量测定是当下研究的热点和难点，可以通过分光光度法、分子排阻-蒸发光散射检测法(SEC-ELSD)、液质联用法(LC-MS)直接测定，也可以水解后法经液相色谱-紫外检测法(HPLC-UV)或气相色谱法(GC)间接测定。但由于聚山梨酯80为聚氧乙烯聚合数目不同的混合物、不同厂家生产的聚山梨酯80化学组分及比例存在较大差异，难以采用统一的转换公式或对照品准确定量。此外，中药注射剂的复杂基质造成的假阳性干扰也对定量提出了挑战。为解决以上问题，以生脉注射液为例，提出基于吸收系数的中药注射剂中聚山梨酯80含量测定新方法。优化检测波长、显色剂种类、液液萃取过程振荡和静置时间，在6个不同品牌仪器上测得聚山梨酯80-硫氰酸钴配合物的吸收系数(E1%_{1 cm})为104.23，相对标准偏差(RSD)为2.08%。生脉注射液稀释10倍后，精密量取供试品溶液1.0 mL，精密加入硫氰酸钴溶液10 mL，二氯甲烷20 mL，涡旋振荡3 min。将混合液移至分液漏斗中，静置30 min，取下层二氯甲烷液，将前1 mL弃去，接收约15 mL，在320 nm处测定吸光度，再根据Lambert-Beer定律，利用获得的吸收系数计算得到聚山梨酯80的含量。方法阴性无干扰，精密度和重复性相对标准偏差均低于3%，平均回收率为98.42%。为进一步验证方法的准确性，分别采用吸收系数法和标准曲线法测定了2个厂家的10批生脉注射液，并与实际投料量比较。配对t检验结果表明，当置信度为95%时，两种方法无显著性差异，吸收系数法测得结果与企业生产中聚山梨酯的实际投料量也无显著性差异。研究采用前人未采用的、灵敏度更高的320 nm为检测波长，显著降低了基质干扰，克服了中药注射剂中聚山梨酯80测定结果与实际投料量难以吻合的问题。吸收系数法无需使用对照品，亦不用制备标准曲线，可为中药注射剂中聚山梨酯80的检查标准提供切实可行的解决方案。所建方法灵敏、准确、快速、简便，为含聚山梨酯80制剂的质量控制提供了关键常数及新的思路。     

A New Two‐Dimensional Coordination Polymer of Mercury(II) with very High Thermal Stability

A 2D Hg^II coordination polymer containing ligands 1,2,4‐triazole (Htrz) and thiocyanate, [Hg(μ₃‐trz)(SCN)]_n ( 1 ) has been synthesized and characterized by elemental analysis and IR spectroscopy. The single‐crystal X‐ray data show the coordination number of Hg atoms is four and the ligand trz^? acts as a three‐fold donor. The thermal stability of compound 1 was studied by thermal gravimetric and differential thermal analyses. The composition and formation of the complex in methanol solution were found to be in support of its solid state structure.     

The Jacobian and the Ginzburg-Landau energy

We study the Ginzburg-Landau functional for , where U is a bounded, open subset of . We show that if a sequence of functions satisfies , then their Jacobians are precompact in the dual of for every . Moreover, any limiting measure is a sum of point masses. We also characterize the -limit of the functionals , in terms of the function space B2V introduced by the authors in [16,17]: we show that I(u) is finite if and only if , and for is equal to the total variation of the Jacobian measure Ju. When the domain U has dimension greater than two, we prove if then the Jacobians are again precompact in for all , and moreover we show that any limiting measure must be integer multiplicity rectifiable. We also show that the total variation of the Jacobian measure is a lower bound for the limit of the Ginzburg-Landau functional. Received: 15 December 2000 / Accepted: 23 January 2001 / Published online: 25 June 2001     

Polyèdre de Newton et distributionf + s . II

Sans résumé

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Chalcogenide based all-solid-state thin electroplated ion-selective membrane for Hg(II) flow-injection determinations

The response to Hg(II) of a thin all-solid-state Te-doped silver chalcogenide membrane, described by the general formula Ag₂ + δSe_{1 − x}Te_x, which has been electrochemically prepared following a previously proposed approach, has been investigated. The kinetics of formation of the membrane's secondary dynamic response to Hg(II) has been successfully combined with the precise timing and transient signal, typical for flow-injection (FI) measurements, in developing a sensitive and reliable mercury FI detector. Under optimized stream conditions it exhibits a linear Nernstian response, with a double slope of the calibration graph of 59 mV dec⁻¹, over the mercury(II) concentration range 10⁻⁶ − 10⁻³ M, the typical sample throughput amounting to about 70 samples per hour. The observed chemical amplification of the signal is due to the specificity of the processes dominating the initial step in formation of the steady-state signal of the membrane to mercury. The analytical performance of the Hg(II) FI detector, as regards sensitivity, reproducibility, selectivity and long-term stability has been thoroughly investigated. The exact procedure for membrane electrodeposition is given and the potential of the proposed approach as a cost-effective way for preparing chalcogenides of unique structure and properties has been outlined in the above context.     

Lévy processes and their subordination in matrix Lie groups

Lévy processes in matrix Lie groups are studied. Subordination (random time change) is used to show that quasi-invariance of the Brownian motion in a Lie group induces absolute continuity of the laws of the corresponding pure jump processes. These results are applied to several examples which are discussed in detail.     

Surface morphologies of anthracene single crystals grown from vapor phase

The morphologies and lattice structures of anthracene single crystals grown from the vapor phase were investigated using optical microscopy, phase contrast microscopy, atomic force microscopy (AFM), and X-ray diffraction analysis. Common morphologies with hexagonal large planes were observed irrespective of crystal size. The observation of certain surface morphologies with a phase contrast microscopy revealed that the spiral steps originated from screw dislocations present on the (0 0 1) planes. Moreover, the center and edge of the (0 0 1) planes had large curvatures, similar to hills. Resultantly, quarter-monolayer (ML) steps were observed on the large and flat planes between both hills.     

On the Hausdorff dimension of generalized Besicovitch-Eggleston sets of d-tuples of numbers

We give a systematic and detailed account of the Hausdorff dimensions of sets of d-tuples of numbers defined in terms of the asymptotic behaviour of the frequencies of strings of digits in their N-adic expansion.     

电感耦合等离子体原子发射光谱法测定化妆品中砷、铅、汞

本文采用五氧化二钒作催化剂，HNO3－H2SO4消解法对化妆品前处理后，用电感耦合等离子体发射光谱仪同时测定砷，铅，汞，方法简便，快速，回收率在95％－103．5％之间，相对标准偏差不大于3％。