核磁共振法快速检测肝素钠粗品

采用1 H NMR对肝素钠、多硫酸软骨素标准品进行测试,并对谱图进行了归属,建立了核磁共振法快速检测肝素钠粗品的分析方法。结果表明:用500MHz核磁共振波谱仪器进行检测,样品浓度为35mg/0.6mL时,能快速(5min)检测出粗品肝素钠中是否存在杂质多硫酸软骨素,检出限为0.3%。     

硫酸软骨素A的解离常数及其金属配合物稳定常数的测定

硫酸软骨素A(ChSA)是葡萄糖醛酸和半乳糖胺通过β-1,3糖苷键所形成的二糖为基本单位的大分子酸性粘多糖。它广泛存在于人及脊椎动物血管及其它脏器结缔组织之中,有关它的生理功能及其在医药等领域中的用途,文献亦有报导。我们曾以镇江肉联厂生产的硫酸软骨素粗品为原料,精制得到纯度较高的硫酸软骨素A制品,并经阳离子交换树脂转化为氢型,测定了它与Cu²⁺、Ca²⁺离子的结合度。     

电感耦合等离子体质谱法测定肝素钠中硼含量

肝素钠是由猪或牛的肠粘膜中提取的硫酸氨基葡聚糖的钠盐,是一种天然抗凝血剂。它广泛用于手术前后防治血栓的形成和作为保存新鲜血液的抗凝剂。原料粗品肝素钠经氧化除杂质后,通常还需通过还原反应来提高产品效价。在这些反应中,常采用硼氢化钾或硼氢化钠作为还原剂,反应后在产     

脱水糖苷化方法合成肝素酶底物寡糖

乙酰肝素酶（Heparanase,Hpa）是哺乳动物体内的内切葡萄糖醛酸苷水解酶,通过水解葡萄糖醛酸（GlcA）与己胺糖（GlcN）之间的β-糖苷键,选择性地降解肝素和硫酸肝素糖胺聚糖,从而释放多功能的肝素寡糖.本文报道一条高效的肝素酶底物寡糖的合成路线：采用苯甲酰基保护待硫酸化的羟基,苄基保护羧基和裸露的羟基,叠氮基保护氨基,应用脱水糖苷化方法高效地构建关键的a-GlcN-（1→4）-GlcA糖苷键.然后通过标准化的保护基脱除和硫酸化操作,获得肝素酶底物三糖和四糖1-4.最后五步反应的总收率超过52%.肝素酶底物寡糖的合成为研究肝素酶的底物选择性和活性检测打下了基础.     

反相高效液相色谱-蒸发光散射检测法测定复方中的盐酸葡萄糖胺

建立了应用反相高效液相色谱-蒸发光散射检测器(RP-HPLC-ELSD)测定复方产品中盐酸葡萄糖胺含量的方法。该方法以C18色谱柱为固定相,甲醇-0.3%五氟丙酸为流动相,采用蒸发光检测器,测定了复方中盐酸葡萄糖胺的含量。结果表明,盐酸葡萄糖胺在0.2～1.0 mg/mL的质量浓度范围内二次回归的相关系数为0.9999,精密度(以相对标准偏差表示)为0.50%。该方法具有简便、快速、准确、重现性较好的特点。     

伯胺N1923从硫酸介质中萃取La（Ⅲ）和Fe（Ⅲ）的动力学

伯胺N1923(以下简称RNH_2)是分离钍和稀土的有效萃取剂。N1923对铁(Ⅲ)和稀土(Ⅲ)萃取热力学的研究表明,在硫酸体系中加入PO_4~(3-),可使稀土(Ⅲ)和铁(Ⅲ)的分离系数增大,本文研究了N1923从硫酸介质中萃取稀土(Ⅲ)和铁(Ⅲ)的动力学性质,以推动N1923在稀土工业中的应用。 N1923由上海有机化学研究所提供,伯胺含量>99％,用等当量浓度的硫酸平衡得到实验     

一种应用快速分离蛋白纯化仪检测肝素钠中多硫酸软骨素的方法

<正>申请公布号:CN104198635A申请公布日:2014.12.10申请人:南京健友生化制药股份有限公司摘要:本发明公开了一种应用快速分离蛋白纯化仪检测肝素钠中多硫酸软骨素的方法。本发明采用具有紫外检测器和电导检测器的快速分离蛋白纯化仪和强阴离子交换色谱柱     

N-乙酰葡萄糖胺的性质、制备及用途

介绍N-乙酰葡萄糖胺的性质、制备和用途,尤其是在医学上的用途。     

国产胺型萃取剂N-1923在钍的分析化学中的应用

前言本文对国产胺型萃取剂伯胺N-1923萃取钍的性能进行了试验。证实它是钍的特效萃取剂,特别适用于从大量铁和稀土中分离富集微量钍。高分子胺常被称为“液体阴离子交换剂”,它兼有溶剂萃取和离子交换二者的优越性。它们的特性前人曾做过很多研究工作。从独居石的硫酸分解液中用伯胺萃取分离钍的研究,六十年代初国外已有报导。自1975年以来,我国开始使用国产伯胺进行从包头矿硫酸分解液中萃取除钍的一系列研究工作,证实N-1923萃取分     

葡萄糖及其衍生物的直接紫外检测毛细管区带电泳研究

 发展了在 195nm波长下直接检测葡萄糖及其衍生物的毛细管区带电泳方法。在未涂渍石英毛细管中 ,以 5 0mmol/LNa2 HPO4 5 0mmol/LNaH2 PO4 为缓冲液体系 (接近生理条件 pH 7 4) ,分离了葡萄糖及其衍生物 (葡萄糖胺、N 乙酰葡萄糖胺和葡萄糖酸钠 )。在各自相应的浓度范围内 ,峰面积与样品浓度之间呈现良好的线性关系。方法简单、快速、重复性好 ,为研究葡萄糖及其衍生物与凝集素的相互作用奠定了分离检测的基础。     

Quantitative Analysis of Clove Oil by NMR Spectrometry

A procedure utilizing NMR spectrometry in the quantitative analysis of clove oil is described. The ¹H-NMR spectrum is determined with acetophenone as internal standard, the ¹³C-NMR spectrum is determined with chloroform as internal standard and 0.1M Cr(acac)₃ as relaxation reagent. The contents of eugenol are compared to the results obtained from G.C. (90.8%, s.d. 0.7%) and from chemical method (89.6% s.d. 1.2%). The result obtained from ¹H-NMR method is 90.4% (s.d. 0.3%) and from ¹³C-NMR method is 90.5% (s.d. 0.7%). The time required for the ¹H-NMR method is about 20mins and for the ¹³C-NMR method is about 2-3hours. Apparently the ¹H-NMR method proves to be more simple, rapid and accurate.     

基质分散固相萃取-液相色谱-离子阱质谱法检测罐头食品中双酚类化合物残留

建立了采用基质分散固相萃取-液相色谱四级杆串联线性离子阱质谱分析罐头食品中双酚类化合物残留的方法.样品中的双酚类化合物残留经0.1％甲酸乙腈提取,基质分散固相萃取净化,外标法定量,液相色谱-质谱测定.使用数据相关采集扫描功能(IDA)结合增强离子产物(EPI)模式对样品中的双酚类进行定性分析,并建立双酚类的二级子离子谱库.通过MRM模式对双酚类进行定量分析,双酚类化合物在4种罐头食品中的平均回收率为49.3％～128.4％(n=6);相对标准偏差在3.2％～14.4％(n-6)之间,可以满足对罐头食品中的双酚类残留的快速同时定性与定量检测的要求.     

Direct determination of four fluoroquinolones,enoxacin, norfloxacin,ofloxacin, and ciprofloxacin,in pharmaceuticals and blood serum by HPLC

A rapid, accurate and sensitive method has been developed for the quantitative determination of four fluoroquinolone antimicrobial agents, enoxacin, norfloxacin, ofloxacin and ciprofloxacin, with high in-vitro activity against a wide range of Gram-negative and Gram-positive organisms.A Kromasil 100 C(8) 250 mm x 4 mm, 5 microm analytical column was used with an eluting system consisting of a mixture of CH(3)CN-CH(3)OH-citric acid 0.4 mol L(-1) (7:15:78 %, v/v). Detection was performed with a variable wavelength UV-visible detector at 275 nm resulting in limits of detection: 0.02 ng per 20 microL injection for enoxacin and 0.01 ng for ofloxacin, norfloxacin and ciprofloxacin. Hydrochlorothiazide (HCT) was used as internal standard at a concentration of 2 ng microL(-1). A rectilinear relationship was observed up to 2 ng microL(-1) for enoxacin, 12 ng microL(-1) for ofloxacin, 3 ng microL(-1) for norfloxacin, and 5 ng microL(-1) for ciprofloxacin. Separation was achieved within 10 min. The statistical evaluation of the method was examined by performing intra-day (n=8) and inter-day precision assays (n=8) and was found to be satisfactory with high accuracy and precision. The method was applied to the direct determination of the four fluoroquinolones in human blood serum. Sample pretreatment involved only protein precipitation with acetonitrile. Recovery of analytes in spiked samples was 97+/-6% over the range 0.1-0.5 ng microL(-1).     

衍生化气相色谱法测定盐酸芬氟拉明片的纯度

 应用衍生化气相色谱法测定盐酸芬氟拉明片的纯度。样品溶解后经碱化乙酸乙酯提取 ,以盐酸美西律作内标 ,提取液用三氟乙酸酐进行酰化衍生化 ,衍生化产物在 5 %SE 30的色谱柱上分析 ,用氢火焰离子化检测器 (FID)检测。实验结果表明 ,芬氟拉明的质量浓度在 0 1g/L～ 0 5 g/L范围内线性良好 (r =0 9996 ) ;芬氟拉明与内标美西律的分离度大于 4;理论塔板数以芬氟拉明峰计大于 2 0 0 0 ;方法的精密度好 ,相对标准偏差 (RSD)为 1 4% (n=7) ;平均回收率为 (10 0 2± 2 2 ) % (n =6 ) ;检测限为 8ng。用该方法得到的结果灵敏、准确、重复性好。     

Quantitative determination of incarvillateine in Incarvillea sinensis by solid phase extraction and high performance liquid chromatography

Method for rapid quantitative analysis of incarvillateine in Incarvillea sinensis by high-performance liquid chromatography (HPLC) has been developed. The sample preparation involves solid phase extraction (SPE) with a mixed-mode reversed-phase and cation-exchange cartridge. The linear calibration range for incarvillateine was 0.002-0.5 mg/ml. The limit of detection was 0.35 microg/ml (S/N=3). Intra- and interday precisions were less than 0.36% (n=6) and 1.61% (n=18), respectively. The recovery of incarvillateine was 97.61-102.44% with the relative standard deviation (RSD) ranging from 0.63 to 1.93% (n=3). This method was proposed as a simple, rapid and accurate method for quantitative determination of incarvillateine content in various samples of Incarvillea sinensis collected from different areas of China.     

Diffusion and NOE NMR studies on the interactions of neutral amino-acidate arene ruthenium(II) supramolecular aggregates with ions and ion pairs

The interaction between [RuCl(AA)(cymene)]n supramolecular aggregates (1, AA = alpha-amino-acidate = alpha-aminoisobutyrate; 2, AA = N,N-dimethyl-Gly; 3, AA = Ala; 4, AA = Pro; cymene = 4-isopropyltoluene) and ionic species derived from NBu4PF6 and KPF6 is investigated through diffusion NMR measurements and 19F,1H-hetero-nuclear Overhauser effect spectroscopy experiments in CDCl3 and CD2Cl2. Aggregates containing the -NH2 functionality (1 and 3) interact strongly with NBu4PF6 as demonstrated by the observation of intense nuclear Overhauser effects between the fluorine atoms of PF6(-) and the protons of [RuCl(AA)(cymene)]n. Unexpectedly, diffusion NMR measurements indicate that the average size of the aggregates increases when a small amount of NBu4PF6 is added (Csalt/CRu < 0.1) in CD2Cl2. At higher concentration levels of NBu4PF6 or in CDCl3, NBu4PF6 exerts a destructive effect that reduces the average size of the aggregates. [RuCl(AA)(cymene)]n aggregates with NR-H (4) and NR2 (2) functionalities are little affected by the addition of NBu4PF6. KPF6 also interacts with [RuCl(AA)(cymene)]n aggregates as demonstrated by the fact that it becomes noticeably soluble in CDCl3 and CD2Cl2. Diffusion1H-NMR experiments show that the addition of KPF6 does not markedly alter the average size of [RuCl(AA)(cymene)]n supramolecular aggregates. Interestingly, the average size of PF6(-)-containing supramolecular aggregates is, in some cases, slightly higher than that of the ones that do not contain PF6(-). This was deduced by independent measurements of the hydrodynamic volume of the anion and of the ruthenium complexes by diffusion 19F- and 1H-NMR experiments, respectively.     

An improved method validation for rapid determination of acrylamide in foods by ultra-performance liquid chromatography combined with tandem mass spectrometry

An improved method was validated for the determination of acrylamide in foods using ultra-performance liquid chromatography (UPLC) coupled to eletrospray ionization tandem mass spectrometry (MS/MS) in the present study. This improved method supplies a rapid quantitative procedure of acrylamide with a run time of only 3 min. Results showed a good repeatability (RSD< or =4.5%) with 50, 100, 250, 500 and 1000 microg/kg spiked concentrations in potato crisps in within-day (n=5) and day-to-day (n=10) precision tests. Meanwhile, good recoveries (81.6-99.0%) were obtained with the same spiked concentrations in acrylamide-free cereal samples (n=3). The excellent method validation data and proficiency test results (Z-score: -0.1) of the official Food Analysis Performance Assessment Scheme (FAPAS) suggested that the present quantitative method could be applied for rapid determination of acrylamide in many investigations.     

Rapid and reproducible capillary electrophoretic separation of double-stranded DNA fragments in a simple methyl cellulosic sieving system

Summary A rapid, robust and reproducible method providing excellent separation performance and simplicity using a 0.5% MC-4000 methyl cellulosic sieving medium in DB-1 coated capillaries has been developed. The method is suitable for qualitative comparison of DNA restriction profiles for fragments in the size range 100–1000 base pairs (bp). Efficiencies up to 8.5 million plates/m (1057 bp fragment) were recorded. Peak resolution of 6 bp (291/297 bp, 335/341 bp) and 4 bp (238/242 bp, 341/345 bp) was achieved. In addition, 1 bp partial resolution of 123/124 bp and 298/297 bp was obtained. Run-to-run (n=15), day-to-day (n=4), and capillary-to-capillary (n=3) variations of 0.1–0.2% RSD, 0.3–0.5% RSD, and 0.1–0.3% RSD, respectively, were observed. The MC-4000 sieving matrix was found to be better than hydroxypropyl methyl cellulose and hydroxypropyl cellulose, in terms of both performance and stability in the DB-1 coated capillaries. The efficiency and resolution in DB-WAX capillaries were inferior to those obtained in DB-1 capillaries. The commercially available DB-1 capillaries were stable for months in the sieving medium at pH 8.3 and could be regenerated to provide high efficiency after accidental current breaks.     

液相色谱串联质谱法测定酒类中甜蜜素含量的探讨和改进

对SN／T1948-2007《进出口食品中环基氨基磺酸钠的检测方法液相色谱-串联质谱》中关于酒类中环己基氨基磺酸钠含量测定方法存在的问题进行探讨和改进。使用氮吹仪去除样品中含有的乙醇,通过C18色谱柱进行分离,以0．1％甲酸水溶液-甲醇作为流动相,在ESI负离子模式下检测。环己基氨基磺酸纳含量在10—10（3ng／mL的范围内与峰面积有良好的线性关系,相关系数r=0．9996,检出限为0．01mg／kg。在两个添加水平下,样品的加标回收率分别为99．5％,99．9％,测定结果的相对标准偏差为0．1％（n=6）。改进后的方法准确、可靠,可用于酒类产品中甜蜜素的定量定性检验。     

4，5-环氧-α-紫罗兰酮的合成研究

研究以H2O2为氧化剂,钨酸钠／磷酸／十六烷基氯化毗啶原位合成的过氧钨配合物催化α-紫罗兰酮合成4,5-环氧-α-紫罗兰酮的反应,考察了催化剂用量、反应温度、反应时间、pH值、溶剂及季铵盐等因素对反应的影响。结果表明,以1,2-二氯乙烷作溶剂,nα-紫罗兰酮：n钨酸钠：n磷酸：n十六烷基氯化吡啶：n过氧化氢=100：0.3：0．1：0．2：120,pH值为4．0,65℃的条件下反应6h,收率可达85％,其结构通过MS、^1H-NMR、IR、EA等检测技术进行表征。