复方制剂中诺氟沙星的 HPLC法测定

采用Kromasil C18为分析柱、0．01mol／L磷酸二氢钠液－甲醇（体积比67：33,用磷酸调pH2．4）为流动相、272nm为检测波长,以HPLC外标法测定复方制剂中诺氟沙星的含量。该法能很好地分离测组分和有关杂质,被测组分的线性关系良好,回收率令人满意。该法专属性好,快速、准确。     

高效液相二极管阵列检测法同时测定复方丹参制剂中7个成分的含量

采用高效液相二极管阵列检测法同时测定3种复方丹参制剂中的7个成分:原儿茶醛、丹酚酸B、丹参酮ⅡA、隐丹参酮、三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1。应用Zorbax C18柱,以0.1%磷酸水溶液和乙腈为流动相,梯度洗脱,流速1 mL/m in(22~28 m in,0.8 mL/m in),柱温30℃,检测波长203、270和281 nm。7个成分的峰面积与浓度的线性关系良好(r>0.9992);加样回收率为94.4%~104.9%。该方法简单、准确、重现性好,可为全面评价复方丹参制剂的质量提供依据。     

一种测定中药复方制剂中活性成分的计算分析方法

提出了一种测定中药复方制剂中活性成分含量的计算分析新方法。该方法将主 成分分析和广义秩消因子分析集成用于处理HPLC／DAD数据，并改进了传统的IND因 子指示函数，适用于定量计算分析复杂混和物体系中的待测成分。将其用于测定复 方丹参制剂中三七皂苷R1的含量，计算分析结果表明，本方法明显优于广义秩消因 子法，同时证明IND函数的改进提高了计算分析准确度。     

柱前衍生化高效液相色谱法测定固定剂量复方抗结核制剂中盐酸乙胺丁醇的含量和溶出度

建立了快速、灵敏和准确的柱前衍生化高效液相色谱测定固定剂量复方抗结核制剂中盐酸乙胺丁醇的含量和溶出度的方法。在无水环境下,盐酸乙胺丁醇与苯乙基异氰酸酯发生柱前衍生化反应的最佳反应的物质的量比为1∶6,检测波长为215 nm。该法成功地用于由4种药物组成的复方抗结核制剂中盐酸乙胺丁醇的含量和溶出度的测定。     

基于标准制剂控制模式和定量指纹图谱评价复方甘草片的质量一致性

通过建立复方甘草片标准制剂（SP）控制模式和定量高效液相色谱指纹图谱,结合5个质量标志物的精准定量评价了9个厂家共145批复方甘草片质量一致性。首先建立了复方甘草片标准制剂的标准指纹图谱（SP-RFP）,然后以SP-RFP作为评价标准,采用系统指纹定量法对145批复方甘草片进行整体定性和整体定量评价。用双标校正法校正定量指纹图谱的系统误差,结果表明所检样品质量均合格。此外,在统一化色谱条件下测定各原料药和模拟样品,对制剂指纹进行归属相关度和准确度评判,得到原料指纹与制剂指纹的相关性,从而实现智能预测制剂或原料药质量和阻止低劣原料入药。同时用紫外全指纹溶出度法测定5个厂家的复方甘草片的溶出度曲线,用以评价制剂工艺的合理性。以上方法可行且准确度高,实现了对复方甘草片质量和工艺的一致性评价。该文为中药质量一致性评价提供了基础评价模式和基本操作思路以及具体实例。     

偏最小二乘-一阶导数分光光度法测定苯甲酸复方制剂中苯甲酸及水杨酸的含量

复方苯甲酸涂剂主要成分是苯甲酸和水杨酸,其在临床上常用于治疗皮肤疾患,由于紫外吸收光谱重叠较严重,用光度法测定时,彼此相互干扰。计量学方法的兴起为多组分的同时测定提供了一种不需分离的新技术。偏最小二乘法可以最大程度地从校正试样中提取信息,具有较强的数据处理能力,因而优于主成分回归等其它计量学方法。本工作将导数光谱的高灵敏度与偏最小二乘法的优良解析性能相结合,提出了同时测定两组分的偏最小二乘导数分光光度法,方法用于复方苯甲酸制剂中两组分的测定,对加和性不太好的体系,也能得到较为满意的结果。     

三烃基锡配合物（PhCMe2CH2）3Sn[O2C（CHRPh）][R：OH（1）, H（2）]的合成、结构、热稳定性、量子化学及毒性研究

甲醇中氧化双[三（2-甲基-2-苯基）丙基锡]分别与DL-扁桃酸、苯乙酸反应,合成了2个三烃基锡配合物（PhCMe₂CH₂）₃Sn[O₂CCH（OH）Ph]（1）和（PhCMe₂CH₂）₃Sn（O₂CCH₂Ph）（2）。经IR、¹H和¹³CNMR、元素分析和X-射线单晶衍射表征结构。1和2均属三斜晶系,空间群P1。配合物1晶体学参数：a=0.9711（2）nm,b=1.1766（3）nm,c=1.7008（4）nm,α=96.840（12）°,β=103.235（12）°,γ=110.725（11）°,Z=2,V=1.7260（7）nm³,D_c=1.288g·cm^-3,μ（MoKα）=0.773mm^-1,F（000）=696,R₁=0.0325,wR₂=0.0873。配合物2晶体学参数：a=0.97285（9）nm,b=1.16140（11）nm,c=1.68931（16）nm,α=96.830（5）°,β=101.935（5）°,γ=110.770（4）°,Z=2,V=1.7071（3）nm³,D_c=1.271g·cm^-3,μ（MoKα）=0.778mm^-1,F（000）=680,R₁=0.0248,wR₂=0.0673。1和2的中心锡原子均为畸变四面体构型。通过分子间C-H…O或C-H…π作用,1和2分别形成一维带状或链状结构。热重分析结果表明,1和2具有良好的稳定性。毒性测试的初步结果表明,配合物1、2具有较好的环境相容性,对石螺急性毒性较小。     

Anhydrous Mercurous Chlorate,Hg2(ClO3)2

Colourless single crystals of the anhydrous mercurous chlorate were grown from a solution of mercuric oxide (HgO) in chloric acid (HClO₃) in the presence of elemental mercury. The crystal structure (monoclinic, P2₁/n, Z = 4, a = 816.59(12), b = 641.02(5), c = 1290.3(2) pm, β = 97.506(12)°, R(all) = 0.0317) contains trans‐O₂ClO‐Hg‐Hg‐OClO₂ molecules with a Hg‐Hg distance of 251.03(4) pm, Hg‐O (bond) distances of 218 and 224 pm and Hg‐Hg‐O angles of 177 and 165°, respectively.     

Hg2(OH)[BF4], the First Basic Mercurous Tetrafluoroborate

The first basic mercurous tetrafluoroborate, Hg₂(OH)[BF₄], was obtained through a synproportionation reaction of red mercuric oxide, HgO, and elemental mercury in a 35% solution of HBF₄ in water as colourless single crystals. The crystal structure (orthorhombic, Pbca, Z = 8, a = 985.0(1), b = 991.0(1), c = 1141.0(2) pm) contains [(HO)_1/2—Hg—Hg—(OH)_1/2]⁺ zig‐zag chains that are further connected via weak Hg—OH interchain interactions to layers between which the [BF₄]^— are located in an up and down fashion.     

Strong Attraction of Caffeine to the Mercurous Dumbbell in the Salt [Hg2(Caf)2](ClO4)2(H2O)2

Colourless single crystals of the caffeine adduct of mercurous perchlorate dihydrate, [Hg₂(Caf)₂](ClO₄)₂(H₂O)₂, were grown from aqueous solutions of mercurous perchlorate and caffeine by isothermal evaporation at ambient temperature. The crystal structure (monoclinic, P2₁/n, Z = 4, a = 1628.0(2), b = 780.4(1), c = 2229.6(3) pm, β = 99.84(1)°, R₁(all data) = 0.0894) contains [trans‐Caf‐Hg‐Hg‐Caf]²⁺ cations with a Hg‐Hg distance of 250.88(6) pm, Hg‐N (bond) distances of 214.4(6) and 215.1(6) pm and Hg‐Hg‐N angles of 176.9(2) and 165.1(2)°, respectively. These cations are attached via weak Hg‐O contacts to dimers which are further arranged to leave large channels into which one crystal water molecule is included. The second water molecule and the two perchlorate anions are weakly attracted to one Hg atom.     

Single Crystal Growth and Crystal Structure of Mercurous Diarsenate(V), (Hg2)2(As2O7)

Polycrystalline mercurous diarsenate(V), (Hg₂)₂(As₂O₇), was prepared by a redox‐reaction between stoichiometric amounts of HgO and As₂O₃. Canary yellow single crystals were obtained by subsequent chemical transport reactions using HgCl₂ as transport agent [550 → 500 °C, 5 d, sealed and evacuated silica ampoules]. The crystal structure (orthorhombic, Pnma, Z = 4, a = 9.9803(8), b = 12.2039(10), c = 7.2374(6)Å) is composed of two crystallographically independent Hgequation/tex2gif-stack-1.gif dumbbells (d¯(Hg—Hg) = 2.5133Å) with a symmetric oxygen coordination sphere, and a diarsenate group with a staggered conformation and a bent bridging angle As—O—As = 121.0(7)°. The building units are arranged in a layer‐like assembly parallel to (010) and are connected via common oxygen atoms to form a three‐dimensional network.     

复方黄芩滴鼻液的制备与临床应用

复方黄芩滴鼻液对过敏性鼻炎有确切疗效，通过对２７例过敏性鼻炎患者观察，２０例有效，５例好转，且无毒副作用，药效高，安全可靠，又因含有人体必需的微量元素及维生素等，而增加了机体的免疫力，使治愈效果增加。     

M(benzo‐18‐crown‐6)I4 (M = Cd,Hg): Tetraiodide,Iodide–Iodine Adduct,or an Inclusion Compound of Iodine in MI2@(benzo‐18‐crown‐6)?

M(benzo‐18‐crown‐6)I₄ (M = Cd, Hg) are obtained as red columnar crystals from the reactions of benzo‐18‐crown‐6 (b18c6), cadmium and mercury iodide, respectively, and iodine in molar ratios of 1:1:2 in acetonitrile. They both crystallize with the orthorhombic crystal system, P2₁2₁2₁, a = 833.7(1), b = 1610.9(1), c = 1846.8(1) pm, V = 2480.3(1) 10⁶·pm³, Z = 4, for M = Cd and a = 823.4(1), b = 1616.5(1), c = 1866.1(1) pm, V = 2483.8(2) 10⁶·pm³ for M = Hg. The crystal structures consist of [M(b18c6)]I₂ molecules which are connected to a slightly lengthened iodine molecule via a secondary contact, according to the formulation I₂@[MI₂@(b18c6)].     

GC-MS技术在舰船复合板毒性评价中的应用

海军舰船舱室多为密闭环境,其舱室狭小,设备庞杂,人员密集。舱室内部的防护装饰多系非金属材料,随着现代各种复合、聚合材料的迅速发展和广泛使用,周围环境特别是密闭舱室空气污染的问题也更为突出。本文根据有关军用标准和规程[1],应用GC-MS技术对2种舰船复合板常温释放物和高     

Nanometer Channels and Cages within the Extended Basic Mercurous Cations [(Hg2)3(OH)2]4+ and [(Hg2)2O]2+

The two‐ and three‐dimensional mercurous cations [(Hg₂)₃(OH)₂]⁴⁺ and [(Hg₂)₂O]²⁺ crystallize with channels and cages of roughly 1 nm diameter from aqueous solutions dependent upon the acidity of the solution. Crystal structures were determined, for example, for [Zn(H₂O)₆][(Hg₂)₃(OH)₂](NO₃)₆ (trigonal, space group P321, a = 1183.5(2) pm, c = 534.8(1) pm, Z = 1, R1 = 0.0351 for I₀ > 2σ(I₀)) and for [(Hg₂)₂O][Pb(NO₃)₃]₂ (cubic, space group , a = 1543.1(2) pm, Z = 8, R1 = 0.0534 I₀ > 2σ(I₀)).     

The Synthesis and Molecular Structure of the First Two-Coordinate,Dinuclear σ-Bonded Mercury(I) RHgHgR Compound

A linear Si-Hg-Hg-Si arrangement and a Hg–Hg distance of 265.69 pm are exhibited by the first two-coordinate, dinuclear σ-bonded organomercury(I ) compound 1. It was formed unexpectedly in the reaction of two equivalents of the silane (Me₃SiMe₂Si)₃SiH with tBu₂Hg. In contrast if the reagents are allowed to react in a 1:1 ratio the expected mercury(II ) compound (Me₃SiMe₂Si)₃SiHgtBu is obtained.