不同色谱柱测定乙酰螺旋霉素原料及其制剂中各组分的含量

目的:对《中国药典》2005年版乙酰螺旋霉素原料及其制剂组分测定方法中"系统适用性"的控制要求进行修订。方法:以标准品图谱为标准,采用4款C18填料的色谱柱对4个厂家22个批次的原料及其制剂进行各组分的含量测定和分离度、柱效的考察。结果与结论:在原要求下,同一样品可因分离情况不同而导致测定结果的差异;只有在样品测定时记录的色谱与标准图谱中各组分的保留时间、分离杂质个数和杂质的基线分离完全一致的情况下,即以现行批乙酰螺旋霉素标准品的标准图谱作为"系统适用性"的控制,才可以保证测定结果的准确。     

舟山眼镜蛇毒细胞毒素的分离纯化及其体外抗肿瘤活性

目的从眼镜蛇毒中分离纯化细胞毒素 F(CTX F)并鉴定其活性。方法应用凝胶过滤、离子交换柱色谱及疏水柱色谱等方法从舟山眼镜蛇毒中分离纯化CTX F ,以SRB法观察CTX F对体外培养癌细胞的杀伤作用。结果眼镜蛇毒粗毒经凝胶过滤获得 4个蛋白峰 ,将CTX所在第Ⅳ峰用阳离子交换柱色谱获A、B、C、D、E、F和G等7个组分 ,其中E、F和G具CTX活性 ,将F组分再经凝胶过滤和疏水色谱进一步纯化得不含磷酯酶A2 (PLA2 )的CTX纯品 ,暂定名为CTX F ,它对多种癌细胞株有杀伤作用。结论应用凝胶过滤、离子交换和疏水色谱等方法可从眼镜蛇毒中获得不含PLA2 的CTX ,其组分F有抗肿瘤活性     

浅谈薄层色谱法鉴别乙酰螺旋霉素

乙酰螺旋霉素(acetyl spriamycin.Ac-Spm)是大环内脂类抗生素螺旋霉素的乙酰化衍生物.严格地说它是一种混合物,其组分为:单乙酰螺旋霉素Ⅱ、单乙酰螺旋霉素Ⅲ、双乙酰螺旋霉素Ⅱ、双乙酰螺旋霉素Ⅲ.     

色谱柱参数对盐酸四环素有关物质HPLC分析的影响研究

摘要：目的 分析色谱柱参数对盐酸四环素有关物质HPLC分析的影响，筛选影响关键杂质分离度以及理论塔板数的主要 柱参数。方法 针对《中国药典》2020版中盐酸四环素有关物质检查的色谱条件，使用多个品牌不同型号的色谱柱进行色谱分 析，使用SPSS软件进行模型回归，得到柱参数与目标因子分离度及理论塔板数的回归方程，并用实测值进行验证。结果 色谱 柱参数C是影响杂质4-差向四环素和土霉素分离度(R12)的重要参数，利用柱参数C可快速预测不同色谱柱的相似度，进而筛选 适宜四环素分析的色谱柱；探讨了金霉素理论塔板数(R5N)与柱参数之间的关系，其中参数B2对R5N影响较大。结论 建立柱参 数与色谱分析目标因子之间的联系，为盐酸四环素有关物质测定选择合适的色谱柱提供便利与指导。     

色谱柱柱长的选用对一检品检验成本的影响

目的　探讨色谱柱柱长的选用对一检品———小儿豉翘清热颗粒检验成本的影响。方法　用HPLC法测定小儿豉翘清热颗粒中栀子苷含量 ,用不同型号色谱柱来测定 ,进行柱效、分离度、含量的对比 ,进行成本核算。结果　No .0 4 74 0 1柱较No.2 13133柱每月 (生产 30批计 )可节约检验成本 2 0 0 0元左右。结论　经过实践 ,在本制剂的含量测定中No .0 4 74 0 1柱比No .2 13133柱更适用     

蜜炙黄芪的化学成分研究

目的研究蜜炙黄芪的化学成分。方法采用大孔吸附树脂柱色谱、硅胶柱色谱、制备薄层色谱、重结晶、凝胶柱色谱、HPLC制备柱色谱等手段，以体积分数70％乙醇提取，从蜜炙黄芪中分离得到7个化合物：利用理化性质和波谱学分析鉴定它们的化学结构。结果与结论分离鉴定了7个皂苷类化合物，分别为大豆皂苷Ⅰ甲酯（1）、黄芪皂苷Ⅰ（2）、黄芪皂苷Ⅱ（3）、异黄芪皂苷I（4）、异黄芪皂苷Ⅱ（5）、黄芪皂苷Ⅲ（6）、β-胡萝卜苷（7）。化合物1为首次从该种植物中分离得到的已知化合物。     

高效液相色谱法分离小诺霉素及其有关的组份

本文叙述了反相高效液相色谱法分离小诺霉素和庆大霉素C组份的一系列色谱系统。用μBondapak C_(18)柱或Radial-pak C_(18)径向加压柱,选择不同的流动相,采用柱前或柱后邻苯二甲醛衍生化技术,荧光或紫外检测器检测,得到几组色谱分离图谱,可使小诺霉素和庆大霉素主要组份在20min内同时得到分离。该条件还适于紫苏霉素和威大霉素的分离和测定。     

提升超高压液相色谱柱温对分离人参皂苷的影响

温度是影响超高压液相色谱(UHPLC)柱效率和背压的主要因素之一。此项研究的目的是监测在用 UHPLC 分离人参皂苷过程中,温度和流动相对柱效率和分离基本要素的影响。UHPLC 采用 JASCO X-LC 系统,Jasco X-PressPak C_(18) S 柱(50 mm×2.1 mm,2.0μm)和Jasco ODS C_(18)柱(50 mm×2.1 mm,1.8 μm)。色谱条     

色谱柱柱长的选用对一检品检验成本的影响

目的 探讨色谱柱柱长的选用对一检品——小儿豉翘清热颗粒检验成本的影响。方法 用HPLC法测定小儿豉翘清热颗粒中栀子苷含量，用不同型号色谱柱来测定，进行柱效、分离度、含量的对比，进行成本核算。结果 No．047401柱较No．213133柱每月(生产30批计)可节约检验成本2000元左右。结论 经过实践，在本制剂的含量测定中No．047401柱比No．213133柱更适用。     

色谱柱柱长的选用对一检品检验成本的影响

目的探讨色谱柱柱长的选用对一检品——小儿豉翘清热颗粒检验成本的影响。方法用HPLC法测定小儿豉翘清热颗粒中栀子苷含量,用不同号色谱柱来测定,进行柱效、分离度、含量的对比,进行成本核算。结果NO.047401柱较NO.213133柱每月(生产30批计)可节约检验成本约2000元左右。结论经过实践,在本制剂的含量测定中NO.047401柱比NO.213133柱更适用。     

Studies on acetylspiramycin. 1. Separation and chemical structures of acetylspiramycin components

1. A macrolide antibiotic acetylspiramycin (ASPM) was separated into seven fractions using high performance liquid chromatography (HPLC) with Lichrosorb RP-8 and mobile phase of a mixed solvent of 0.025M phosphate ammonium (pH 7.4) and acetonitrile at a ratio of 10:18. 2. Five components were purified over 90%, and analyzed using mass spectroscopy, 1H NMR, and 13C NMR, and their chemical structures were determined as 4'-acetylspiramycin I, 4'-acetylspiramycin II, 4'-acetylspiramycin III, 3',4'-diacetylspiramycin II and 3',4'-diacetylspiramycin III, respectively. 3. The weight component ratio of the seven fractions of ASPM separated by HPLC was constant throughout several lots of ASPM which had been stocked for nearly 15 years at room temperature, indicating an excellent chemical stability of the antibiotic. 4. Some physicochemical parameters were determined for the five ASPM components. Solubilities in water at 24 degrees C were in a range from 0.14 mg/ml to 4.9 mg/ml, and they were, in the decreasing order, 3',4'-diacetylspiramycin III, 3',4'-diacetylspiramycin I 4'-acetylspiramycin III, 4'-acetylspiramycin II, and 4'-acetylspiramycin I. Relationships between solubilities and numbers and positions of acyl substituents in spiramycin molecule are discussed.     

Column selection for pharmaceutical analyses based on a column classification using four test parameters

This paper focuses on the usability of a previously developed column classification system, applied to pharmaceutical analyses. The separation of two drugs from their respective related substances was investigated on 65 new reversed-phase liquid chromatographic columns. The chromatographic procedure for fluoxetine hydrochloride was performed according to the method prescribed in the European Pharmacopoeia monograph while the separation of gemcitabine hydrochloride was carried out according to the United States Pharmacopeia monograph. It was shown that the column ranking system is a helpful tool in the selection of a suitable column.     

手性色谱柱用于天冬中甾体皂苷类似物的分离

天冬是一味以甾体皂苷为主要活性成分的常用中药。由于其甾体皂苷同系物及同分异构体的存在,在采用正相硅胶与反相ODS柱色谱相结合的方法进行分离时,有些同系物无法有效分离。本实验系统地筛选了不同分离机制的色谱柱,意外地发现纤维素类型的手性色谱柱能够有效分离这些成分,并应用该类型色谱柱对3个混合物进行分离,得到6个单体化合物(1～6)。结构鉴定结果显示,这些较难分离的同系物在结构上的共同差异仅在于C-3位糖链中一个末端糖基的不同(木糖或鼠李糖),并且分离得到的化合物4、6为两个新甾体皂苷。由于在分离纯化天然产物时被分离化合物的结构未知,很少使用手性色谱柱进行分离。该研究提示对于常规难以分离的天然产物,手性色谱柱也是一个重要选择。     

基于溶解氧乙酰螺旋霉素极谱平行催化氢波的研究

目的提出一种极谱测定乙酰螺旋霉素(ASPM)的新方法。方法应用单扫描极谱法,在含溶解氧的0.1 mol·L^-1 NH₄Cl-NH₃·H₂O(pH 8.9)缓冲液中ASPM产生1个灵敏的平行催化氢波［峰电位E_p=-1.63 V(vs SCE)］。结果该平行催化氢波的二阶导数峰峰电流i″与ASPM浓度在1.74×10^-3～3.48 μg·mL^-1呈良好线性关系(r=0.997 9,n=13),检出限为5.80×10^-4 μg·mL^-1(3σ)。对0.871 μg·mL^-1 ASPM溶液进行13次平行测定,RSD为1.24%。结论本方法可用于ASPM片剂中ASPM含量的测定。     

流动注射化学发光法测定人尿液中纳克水平乙酰螺旋霉素

目的建立流动注射抑制化学发光测定乙酰螺旋霉素的新方法。方法在碱性介质中乙酰螺旋霉素能强烈抑制luminol-K₃Fe(CN)6化学发光反应。本文以乙酰螺旋霉素在一定浓度范围内与luminol-K₃Fe(CN)6化学发光强度降低值的呈线性关系为基础,结合流动注射技术,快速测定乙酰螺旋霉素。结果测定的线性范围为0.1～100 μg·L^-1,检测限为40 ng·L^-1(3σ),RSD小于3.0%(n=8)。结论该法简便快速、灵敏度高、选择性好,可用于药物、人血清中的乙酰螺旋霉素含量的测定,监测口服乙酰螺旋霉素后人尿液中乙酰螺旋霉素的排泄状况。     

Gas uptake in a three-generation model geometry with a flat inlet velocity during steady inspiration: comparison of axisymmetric and three-dimensional models

Mass transfer coefficients were predicted and compared for uptake of reactive gas system using an axisymmetric single-path model (ASPM) with experimentally predicted values in a two-generation geometry and with a three-dimensional computational fluid dynamics model (CFDM) in a three-generation model geometry at steady inspiratory flow with a flat inlet velocity profile. The flow and concentration fields in the ASPM were solved using Galerkin's finite element method and in the CFDM using a commercial finite element software FIDAP. ASPM predicted average gas phase mass transfer coefficients within 25% of the experimental values. Numerical results in terms of overall mass transfer coefficients from the two models within each bifurcation unit were compared for two different inlet flow rates, wall mass transfer coefficients, and bifurcation angles. The overall mass transfer coefficients variation with bifurcation unit from the ASPM and CFDM compared qualitatively and quantitatively closely at lower wall mass transfer coefficients for both 40 degree and 70 degree bifurcation angles. But at higher wall mass transfer coefficients, quantitatively they were off in the range of 2-10% for 40 degree bifurcation angle and in the range of 4-15% for 70 degree bifurcation angle. Both CFDM and ASPM predict the same trends of increase in mass transfer coefficients with inlet flow, wall mass transfer coefficients, and during inspiration compared to expiration. Higher mass transfer coefficients were obtained with a flat velocity profile compared to a parabolic velocity profile using ASPM. These results validate the simplified ASPM and the complex CFDM.     

Gas Uptake in a Three-Generation Model Geometry with a Flat Inlet Velocity During Steady Inspiration: Comparison of Axisymmetric and Three-Dimensional Models

Mass transfer coefficients were predicted and compared for uptake of reactive gas system using an axisymmetric single-path model (ASPM) with experimentally predicted values in a two-generation geometry and with a three-dimensional computational fluid dynamics model (CFDM) in a three-generation model geometry at steady inspiratory flow with a flat inlet velocity profile. The flow and concentration fields in the ASPM were solved using Galerkin's finite element method and in the CFDM using a commercial finite element software FIDAP. ASPM predicted average gas phase mass transfer coefficients within 25% of the experimental values. Numerical results in terms of overall mass transfer coefficients from the two models within each bifurcation unit were compared for two different inlet flow rates, wall mass transfer coefficients, and bifurcation angles. The overall mass transfer coefficients variation with bifurcation unit from the ASPM and CFDM compared qualitatively and quantitatively closely at lower wall mass transfer coefficients for both 40° and 70° bifurcation angles. But at higher wall mass transfer coefficients, quantitatively they were off in the range of 2–10% for 40° bifurcation angle and in the range of 4–15% for 70° bifurcation angle. Both CFDM and ASPM predict the same trends of increase in mass transfer coefficients with inlet flow, wall mass transfer coefficients, and during inspiration compared to expiration. Higher mass transfer coefficients were obtained with a flat velocity profile compared to a parabolic velocity profile using ASPM. These results validate the simplified ASPM and the complex CFDM.     

Gas uptake in a three-generation model geometry during steady expiration: comparison of axisymmetric and three-dimensional models

Mass transfer coefficients were predicted and compared for uptake of a formaldehyde-air gas system using an axisymmetric single path model (ASPM) and a three-dimensional computational fluid dynamics model (CFDM) in three-generation model geometry at steady expiratory flow. The flow and concentration fields in the ASPM were solved using Galerkin's finite-element method and in the CFDM using a commercial finite-element software, FIDAP. Numerical results were compared for two different inlet flow rates, wall mass transfer coefficients, and bifurcation angles. The mass transfer coefficients variation with bifurcation unit from the ASPM and CFDM compared qualitatively and quantitatively closely at all flows and lower wall mass transfer coefficients for both 40 degrees and 70 degrees bifurcation angles. However, at higher wall mass transfer coefficients, quantitatively they were within 40% for both the bifurcation angles. Also, at higher flow and wall mass transfer coefficients, they were off qualitatively for a 70 degrees bifurcation angle although the uptake compared qualitatively. This is due to the normalization of uptake within a bifurcation unit with the average of inlet and outlet average concentrations. Both CFDM and ASPM predict the same trends of increase in mass transfer coefficients with inlet flow and wall mass transfer coefficients. Also, the local values of the mass transfer coefficients compared closely at all conditions. These results validate the simplified ASPM and the complex CFDM. Mass transfer coefficients increase with bifurcation angles and with a flat inlet velocity profile compared to a parabolic velocity profile since the flow is non-fully developed and hence, the uptake increases.     

反相C_(18)液相色谱柱选择性理论及其应用

反相HPLC分析中色谱柱的选择性受到了越来越多的关注,在这些色谱柱中,C18柱是目前最常用的色谱柱,然而各种C18色谱柱在分离效果上也存在着较大差异,因此能否找到合适的C18柱关系到整个实验的成败。经过近年来的研究,已形成了一些色谱柱分类、选择方法,如色谱柱参数(H,S,A,B,C)法、相似系数(F值)法等,减少了色谱柱选择的盲目性。本文结合近年来的研究,归纳了这些方法的优点及其在应用过程中的局限性,并基于前人的理论,结合实际工作,为药品分析中合理选择色谱柱提出了建议和方法。