高速逆流色谱分离纯化防风中升麻素苷和5-O-甲基维斯阿米醇苷

建立了高速逆流色谱分离制备防风中有效成分升麻素苷和5-O-甲基维斯阿米醇苷的方法.防风根的粉末经甲醇浸泡提取和减压蒸馏,得粗提浸膏.以V(乙酸乙酯):V(正丁醇):V(水)=2:7:9为溶剂,上相为固定相,下相为流动相,流速2.0 mL/min.从316 mg防风粗提物中一步分离得到13.9 mg升麻素苷和25 mg 5-O-甲基维斯阿米醇苷,纯度分别为98.1%和99 2%.采用ESI-MS, 1H NMR 和13C NMR对目标化合物的结构进行了鉴定.     

液相色谱-串联质谱法测定农吉利中的黄酮类化合物

采用液相色谱-串联质谱法对农吉利中黄酮化合物进行定性和定量分析。农吉利干药材粉碎后,用甲醇提取,提取液经D101大孔吸附树脂净化后,以UltimateTMC18色谱柱为固定相,以甲醇-0.5%(φ)乙酸混合溶液为流动相进行梯度洗脱,采用电喷雾离子源,分别在正离子和负离子扫描模式下对主要特征碎片离子进行解析。结果表明:提取液中含有牡荆苷、异牡荆苷、荭草苷、异荭草苷和金雀花苷等黄酮类化合物。荭草苷、异荭草苷、牡荆苷和异牡荆苷的质量浓度在一定范围内与其峰面积呈线性关系,检出限(3S/N)分别为50.2,40.5,52.1,42.1μg·L-1。方法应用于农吉利药材的分析,加标回收率在96.0%~103%之间,测定值的相对标准偏差(n=5)小于3.0%。     

HPLC波长切换法同时测定粗茎秦艽中6个成分的含量

本实验建立了HPLC波长切换法同时测定云南丽江粗茎秦艽中马钱苷酸、獐牙菜苦苷、龙胆苦苷、獐牙菜苷、异荭草苷、异牡荆苷6种成分的含量,并对各成分含量间的相关性进行分析,为粗茎秦艽药材质量的全面评价提供了科学依据。采用Sepax Gp-C18(150 mm×4.6 mm,5μm)色谱柱,甲醇-0.1%磷酸为流动相体系,梯度洗脱,流速1.0 mL·min-1,柱温25℃,检测波长235 nm(0~51 min)、270 nm(51~57 min)、243 nm(57~65 min)、270 nm(65~80 min)。马钱苷酸、獐牙菜苦苷、龙胆苦苷、獐牙菜苷、异荭草苷、异牡荆苷的量分别在0.01000~10.0000、0.00216~2.1600、0.0480~48.0000、0.0010~1.0000、0.00034~0.3400、0.00026~0.2600μg范围内与色谱峰峰面积呈良好的线性关系,平均回收率为98.52%~99.31%,RSD均小于3.5%(n=6);对各成分含量间相关性分析发现环稀醚萜苷类与黄酮类组分含量间无相关性,四种环烯醚萜苷类成分的含量之间存在着显著相关性,两种黄酮类成分的含量之间也存在相关性。该方法简便、快速、准确,重现性好,更符合中药材复杂体系的多指标质量控制发展趋势,为粗茎秦艽药材的质量控制找到了简便易行的方法。     

正交设计试验优化高速逆流色谱分离制备玛咖中芥子油苷的条件

基于高速逆流色谱（HSCCC）技术从玛咖中分离制备出两种芥子油苷,苄基芥子油苷（glucotropaeolin, GTL）和甲氧基苄基芥子油苷（glucolimnanthin, GLI）。使用正交设计试验对分离条件进行优化,采用高分辨质谱对制备的组分进行鉴定,采用高效液相色谱法（HPLC）对组分进行定量分析。确定了两个组分GTL与GLI的HSCCC最佳分离条件：溶剂系统为正丁醇-乙腈-200 g/L硫酸铵溶液（1:0.5:2.4, v/v/v）,上相为固定相,下相为流动相,流动相流速2 mL/min,主机转速900 r/min,从玛咖根粗提物中一次性分离得到157.72 mg/kg纯度为97.9%的苄基芥子油苷和31.93 mg/kg的甲氧基苄基芥子油苷,固定相保留率达57.6%。该方法成本低,简便易行,样品损失量小,可大量循环进样制备。     

毛细管电泳法分离测定芦丁、槲皮素和连翘苷

用毛细管电泳紫外检测法同时测定了芦丁、槲皮素和连翘苷，研究了各种条件的影响，得到了优化的实验条件，在20mmol/L的Na2B4O7(H3B03调节至pH8．40)-30mmol/L十二烷基硫酸钠-10％乙腈(1 9)的缓冲溶液中，分离电压为12kV时，芦丁、槲皮素和连翘苷在10min内得到了良好的分离，检测波长为254nm，芦丁、槲皮素和连翘苷分别在0．01-1．0mg/mL，0．01-1．0mg／mL和0．05-1．0mg/mL质量浓度范围内与电泳峰高呈现良好线性关系，检测下限分别为0．005mg/mL，0．005mg/mL和0．01mg／mL，应用于实际样品的测定。     

基于指纹图谱、量值传递及化学计量学的薏苡竹叶散质量评价

建立高效液相指纹图谱进行外部质量控制,结合化学计量学探究内部质量影响因素,通过量值传递规律确定制备工艺稳定性,全面完善薏苡竹叶散（YZP）质量评价系统。利用《中药色谱指纹图谱相似度评价系统》（2012.130723版本）绘制15批YZP指纹图谱并评价相似度;选择Origin 2019b 64Bit进行聚类分析（CA）,利用SIMCA 14.1进行主成分分析（PCA）和正交偏最小二乘判别分析（OPLS-DA）,获得导致质量差异的主要成分;测定15批淡竹叶药材和YZP中荭草苷和异荭草苷的含量,探究样品制备过程中的量值传递规律。结果表明,15批YZP指纹图谱得到21个共有峰,指认了6种成分,分别为9号峰（异荭草苷）、10号峰（荭草苷）、13号峰（牡荆素）、14号峰（异牡荆素）、15号峰（连翘酯苷A）和20号峰（连翘苷）,相似度在0.956～0.995之间,符合相关规定;CA结果显示,15批YZP被分为两类,PCA共得到3个主成分,累计贡献率82.4%,OPLS-DA得出10个贡献率较大成分,包括已指认出的9号峰（异荭草苷）、13号峰（牡荆素）和20号峰（连翘苷）,有利于进一步质量评价;15批...     

金银花不同部位中绿原酸和木犀草苷含量的测定

利用HPLC法测定金银花不同部位中绿原酸和木犀草苷。采用ODS-C18色谱柱(250 mm×4.6 mm,5μm),以甲醇-水(0.03 mol/L磷酸)为流动相进行梯度洗脱,流速:1.0 mL/min,检测波长:350 nm,柱温:室温。绿原酸浓度在0~0.4 mg/mL内与峰面积呈良好线性关系(r2=0.999 6),回收率为101.9%~105.2%,相对标准偏差为3.18%(n=6)。木犀草苷浓度在0~0.1 mg/mL内与峰面积呈良好线性关系(r2=0.999 1),平均回收率为100.5%~104.0%,相对标准偏差为3.42%(n=6)。结果表明:金银花、芽等部位绿原酸和木犀草苷的含量较高。     

加压毛细管电色谱在芎菊上清片中栀子苷及黄芩苷分离检测中的应用

采用加压毛细管反相电色谱技术,建立了一种用于分离检测芎菊上清片中栀子苷和黄芩苷的高效简便新方法。色谱柱为EP-100-20/45-3 C18毛细管柱(总长度45 cm,有效长度20 cm,直径为100μm,ODS填料内径3μm),柱温为25℃,流动相采用20 mmol/L Na H2PO4-乙腈(71∶29),流动相的总流速为0.035m L/min,分离电压为+2.0 k V,检测波长为240 nm。经等度洗脱,栀子苷和黄芩苷可实现快速分离,峰面积的相对标准偏差(RSD)不大于2.8%,回收率为91.9%~101.2%,测得该芎菊上清片中栀子苷的含量为2.616 mg/g,黄芩苷的含量为11.220 mg/g。该方法的选择性好、柱效高、试剂用量少,用于芎菊上清片中黄芩苷和栀子苷的分离检测,结果满意。     

女贞子中红景天苷的HPLC制备分离

研究了制备型高效液相色谱分离纯化女贞子中红景天苷的方法。制备色谱的参数为:色谱柱为C18柱(50 mm×200 mm,5μm),流动相为甲醇-水(体积比为7.5∶92.5),流速100 mL·min-1,二级管阵列检测器在278 nm检测,进样体积为2.2 mL。在18 min的运行时间内,红景天苷与干扰成分得到很好的分离,经HPLC检测纯度均达到98%以上。此方法具有快速高效、分离组分纯度高的特点,可用于制备红景天苷。     

HPLC测定云雾龙胆花中獐牙菜苷和异荭草苷的含量

建立云雾龙胆花中獐牙菜苷和异荭草苷含量测定的HPLC方法。采用微波辅助动态回流法进行提取,色谱条件:Fusion-RP 80 A C18柱(150×4.6 mm,5μm);流动相:甲醇-0.2%磷酸溶液梯度洗脱(0~20 min∶18∶82~30∶70;20~30min∶30∶70~40∶60;30~35min∶40∶60~50∶50);流速:1 mL/min;柱温:30℃;检测波长254 nm。云雾龙胆花中獐牙菜苷和异荭草苷的色谱峰与共存组分完全达到基线分离,线性范围分别为0.25~1.25μg(r=0.9998),0.432~2.160μg(r=0.9999),平均加样回收率分别为97.7%(RSD=0.84%),99.2%(RSD=0.76%)。     

Unified chromatography: Fundamentals,instrumentation and applications†

The concept of unified chromatography has been in existence for 50 years after the work of Giddings proposing that all modes of chromatography (gas chromatography, liquid chromatography, supercritical fluid chromatography and so on) may be treated together under a single unified theory. His idea was partially fulfilled 23 years later by Ishii, Takeuchi and colleagues, who demonstrated for the first time the possibility to analyze a complex sample containing substances with a wide range of boiling points and polarities in the same instrument and column, just by varying the mobile phase pressure and temperature to change from one chromatographic mode to another. This approach has been demonstrated through application to the separation of complex mixtures in several areas including crude oil, edible oils and polymers. Still, unified chromatography has not yet been fully developed. In the present work, we will review the fundamentals, instrumentation and several applications of the technique. Also discussed are the drawbacks that still hinder development, as well as the recent developments and trends in instrumentation and columns that suggest the most feasible ways forward to the full development of unified chromatography.     

高效膜色谱的发展和应用

对新兴的高效膜色谱的基质材料、膜形态、分离机理以及应用进行了综述,并对其用于对映体分离作了展望。共７６篇。     

Extraction chromatography of common anions in liquid-liquid anion exchange systems. Part. III. Monobasic aliphatic organic acids and their sodium salts as eluants

Summary The chromatographic behaviour of anions on paper strips treated with tri-n-octylamine (TOA) salts or Aliquat 336 and developed with aqueous solutions of acetic, formic, monochloroacetic or trifluoroacetic acids and their sodium salts was investigated. Liquid-liquid extraction of organic acids by 0.1 M solution of TOA in benzene as well as the anion exchange between benzene solutions of TOA salts or Aliquat 336 (in acetate form) in benzene and aqueous solutions of sodium halides was also studied. It was found that extraction increases in the following order of the acids: CH₃COOOH<HCOOH<CH₂CICOOH<CF₃COOH; the relative affinity of organic anions to the quaternary alkyl-ammonium cation also increase in a similar order. The extraction of acid in excess over the amount necessary to neutralize the amine was observed for all four acids. The R_F values of anions investigated depend markedly on the type of organic acids or their salts and their concentration in the mobile phase. Halide ions are more strongly retained on paper treated with Aliquat 336 as compared with TOA salts. The chromatographic systems investigated offer many possibilities to separate various anion mixtures.Parts and II: refs. [1, 2].     

流体动力色谱法和障碍色谱法及其应用

介绍了流体动力色谱(HDC)和障碍色谱(SC)及其在生物、化工分离中的研究进展,着重于它们的分离原理、理论发展及二者之间的联系与转化,引用52篇文献.     

Liquid chromatography on unmodified and modified spheron gels I. Nucleosides,bases and related compounds

Summary The ethylene glycol methacrylate gel Spheron and ion exchangers produced by the chemical modification of this gel (such as the cation exchanger Spheron S and anion exchanger Spheron DEAE) are compared with octadecylsilica as column packing materials for reversedphase chromatography of nucleic acid constituents and related compounds. The different separation selectivities of the individual materials can be utilized for the chromatographic separation of these compounds.     

Exhibition of the first gas chromatographic work of Erika Cremer and Fritz Prior

Summary In November 1995, theDeutsches Museum, the world's largest technical museum, opened a new branch in Bonn, devoted to achievements after 1945. There, the first gas chromatographic system used by Erika Cremer and Fritz Prior, in 1945–47, in Innsbruck, is exhibited. The new display is described and the early activities of Erika Cremer and her students are summarized.     

Affinity monolith chromatography: A review of general principles and recent developments

Affinity monolith chromatography (AMC) is a liquid chromatographic technique that utilizes a monolithic support with a biological ligand or related binding agent to isolate, enrich, or detect a target analyte in a complex matrix. The target-specific interaction exhibited by the binding agents makes AMC attractive for the separation or detection of a wide range of compounds. This article will review the basic principles of AMC and recent developments in this field. The supports used in AMC will be discussed, including organic, inorganic, hybrid, carbohydrate, and cryogel monoliths. Schemes for attaching binding agents to these monoliths will be examined as well, such as covalent immobilization, biospecific adsorption, entrapment, molecular imprinting, and coordination methods. An overview will then be given of binding agents that have recently been used in AMC, along with their applications. These applications will include bioaffinity chromatography, immunoaffinity chromatography, immobilized metal-ion affinity chromatography, and dye-ligand or biomimetic affinity chromatography. The use of AMC in chiral separations and biointeraction studies will also be discussed.     

Two dynamic chromatographies and their application

Hydrodynamic chromatography and slalom chromatography known as dynamic liquid chromatography were introduced and reviewed, mainly for the recent development of separation principle, theoretical model, and applications. Fifty-two references were cited.     

Liquid chromatography on unmodified and modified Spheron gels II. Barbiturates and sulfonamides

Summary The ethylene glycol methacrylate gel Spheron and ion-exchangers produced by the chemical modification of this gel (the cation exchanger Spheron S and the anion exchanger Spheron DEAE) can be used for reversedphase chromatography of barbiturates and sulfonamides. In addition to the hydrophobic effect, the unique selectivities of the functional groups of Spheron materials can be utilized for the chromatographic separation of these compounds, including those difficult to resolve on octadecyl silica.Principle author     

Fast and efficient size-based separations of polymers using ultra-high-pressure liquid chromatography

Ultra-high-pressure liquid chromatography (UHPLC) has great potential for the separations of both small molecules and polymers. However, the implementation of UHPLC for the analysis of macromolecules invokes several problems. First, to provide information on the molecular-weight distribution of a polymer, size-exclusion (SEC) columns with specific pore sizes are needed. Development of packing materials with large pore diameters and pore volumes which are mechanically stable at ultra-high-pressures is a technological challenge. Additionally, narrow-bore columns are typically used in UHPLC to minimize the problem of heat dissipation. Such columns pose stringent requirements on the extra-column dispersion, especially for large (slowly diffusing) molecules. Finally, UHPLC conditions generate high shear rates, which may affect polymer chains. The possibilities and limitations of UHPLC for size-based separations of polymers are addressed in the present study. We demonstrate the feasibility of conducting efficient and very fast size-based separations of polymers using conventional and wide-bore (4.6 mm I.D.) UHPLC columns. The wider columns allow minimization of the extra-column contribution to the observed peak widths down to an insignificant level. Reliable SEC separations of polymers with molecular weights up to ca. 50 kDa are achieved within less than 1 min at pressures of about 66 MPa. Due to the small particles used in UHPLC it is possible to separate high-molecular-weight polymers (50 kDa ≤ M(r) ≤ 1-3 MDa, upper limit depends on the flow rate) in the hydrodynamic-chromatography (HDC) mode. Very fast and efficient HDC separations are presented. For very large polymer molecules (typically larger than several MDa, depending on the flow rate) two chromatographic peaks are observed. This is attributed to the onset of molecular deformation at high shear rates and the simultaneous actions of hydrodynamic and slalom chromatography.