无机基质疏水作用色谱填料的研制及扩试

以无机基质可控孔径玻璃（ＣＰＧ）和大孔硅胶为基质、聚乙二醇（ＰＥＧ１０００）为配基,利用改进的合成方法制备了疏水作用色谱（ＨＩＣ）填料,并进行了１５０ｇ／批的扩大试验,用标准蛋白为样品进行了色谱行为的研究。结果表明,此类填料对蛋白质的分离性能良好,对胰蛋白酶的活性回收率大于９５％。     

湘泉酒气相色谱法分析探讨

湘泉酒气相色谱法分析探讨李杜,周继红,詹益兴（湖南教育学院化学系长沙４１００１２）（长沙市化工研究所长沙４１０００７）１实验气相色谱仪：ＧＣ－１４Ａ,ＦＩＤ检测器;色谱柱：ＰＥＧ－２０Ｍ石英交联毛细管柱,５０ｍ×０．２５ｍｍ;柱温：４５℃（５ｍｉｎ）...     

超临界流体色谱法分离手性化合物的进展

超临界流体色谱（ＳＦＣ）是一种很有潜力的色谱分离技术,可以弥补高效液相色谱（ＨＰＬＣ）和气相色谱（ＧＣ）在手性对蚋物分离方面的不足。本文不但介绍了ＳＦＣ仪器的结构特点,ＳＦＣ与手性固定相（ＣＳＰｓ）结合在手性分离领域中的应用和最新进展,还对ＳＦＣ与其它色谱技术的分离效果进行了评价。文献３９篇。     

色谱技术在分离提纯某些立体异构中的应用

色谱技术早巳广泛应用在有机分析上。有关的理论在很多专普及实验书中已有详细阐述。近十多年来在国内外进一步把色谱技术用于有机合成产物的分离提纯上。传统的分离提纯方法是分馏、重结晶、升华等,这些手段难以     

高效液相色谱法测定大白鼠脊髓受到羟基游离基损伤时前列腺素的释放

研究了荧光衍生化试剂Ｂｒ－ＤＭＥＱ与前列腺素（ＰＧＦ２α）的反应条件及其荧光产物的色谱分离条件。方法灵敏度高,最小检测量为１０ｆｍｏｌ。并且利用微透析技术和Ｆｅｎｔｏｎ反应直接在脊髓内产生羟基游离基,测定了中枢神经系统受到羟基游离基损伤时ＰＧＦ２α的释放。     

凝胶色谱法测定顺丁橡胶平均分子量及其分布的研究

通过一系列的条件试验,包括样品浓度、样品量及流动相流速对柱效的影响,确定了最佳的凝胶色谱（ＧＰＣ）试验条件;采用普适校正法将聚苯乙烯（ＰＳ）标定曲线转换成顺丁橡胶（ＰＢ）标定曲线,并对Ｍａｒｋ－Ｈｏｕｗｉｎｋ方程式中Ｋ,α值的选择进行了讨论;采用４种分子量加宽方程对色谱柱加宽效应进行改正计算,通过比较,选定适合本试验系统的加宽效应的改正方法;用粘度法测得的顺丁橡胶特性粘度（η）吻合ＧＰＣ所测得特性粘度值,证明了方法的可靠性。     

石油亚砜馏分的色谱法分离

用经典硅胶柱色谱法将石油亚砜ＰＳＯ分离为４个馏分,对其中的第３个馏分进行了高效制备液相色谱的分离制备。通过大量的试验,建立了较好的色谱条件：以甲醇、水混合液为流动相,以Ｃ_（１８）反相柱为固定相,把ＰＳＯ３分离成７个不同的馏分。对其中的两个馏分ＰＳＯ３_ｃ和ＰＳＯ３_ｅ作进一步的色谱分离和纯化后,获得较纯的亚砜馏分,用作结构分析和性能研究。     

裂解气相色谱—红外光谱联用分析聚合物结构（II）

采用国产ＳＣ－７型色谱以及ＪＰ－０１型居里点裂解器，Ｎｉｃｏｌｅｔ１７０ＳＸ红外光谱仪及接口组成的裂解色相色谱－傅里叶变换红外光谱（ＰＧＣ／ＦＴＩＲ）分析仪，ＨＰ－１７型大口径毛细管色谱柱，分析了两个复杂组成的聚合物样品。从主要裂解碎片峰的定性结果及形成机理出发，逐步推出了原样品的组成和结构，常规红外光谱分析方法被用来作为对比，但它获得的信息有限，无法得到能与ＰＷＢＣＧＣ／ＦＴＩＲ分析结果和媲美的     

裂解气相色谱－红外光谱联用分析聚合物结构（Ⅱ）

采用国产ＳＣ－７型色谱仪及ＪＰ－０１型居里点裂解器、Ｎｉｃｏｌｅｔ１７０ＳＸ红外光谱仪及接口组成的裂解气相色谱－傅里叶变换红外光谱（ＰＧＣ／ＦＴＩＲ）分析仪、ＨＰ－１７型大口径毛细管色谱柱，分析了两个复杂组成的聚合物样品。从主要裂解碎片峰的定性结果及形成机理出发，逐步推出了原样品的组成和结构。常规红外光谱分析方法被用来作为对比，但它获得的信息有限，无法得到能与ＰＷＢＣＧＣ／ＦＴＩＲ分析结果相媲美的结论，充分显示了ＰＷＢＣＧＣ／ＦＴＩＲ用于聚合物分析的优越性。     

反相高效液相色谱法同时测定桑叶提取物中芸香甙和槲皮素的含量

用Ｐ１００型高效液相色谱系统、ＤＬ－８００色谱工作站、ＹＷＧ－Ｃ１８色谱柱,以甲醇－水－磷酸体系（６０∶４０∶０．４,Ｖ／Ｖ／Ｖ）为流动相分离并同时测定了桑叶提取物中芸香甙与槲皮素的含量。芸香甙、槲皮素含量与峰面积呈良好的线性关系。芸香甙的变异系数为１．９８％,回收率为１０４．０％;槲皮素的变异系数为９．８％,回收率为１０３．２％。     

The use of multidimensional chromatography for the isolation of synthetic oligodeoxyribonucleotides on a preparative scale

Summary A critical step in the chemical preparation of oligonucleotides is the chromatographic purification of the deprotected oligomers. In case of large quantities of reaction products, the oligonucleotides are first enriched on a QAE-Sephadex column at low pressure. The obtained fractions are then purified by multidimensional chromatography making use of three independent physical properties of the solutes: molecular size, ionic net charge and hydrophobicity. In the first dimension size exclusion chromatography (Sephadex G-15) is used. In the second dimension the high molecular weight fraction from the size exclusion chromatography is applied to a HPLC ion-exchange column (Partisil-10 SAX). Usually the last peak is collected and transferred to a HPLC reversed phase column (Nucleosil C18) where the components are separated according to their hydrophobicity in the third dimension. The efficiency of this multi-dimensional chromatographic procedure is demonstrated by the unequivocal fingerprints after radioactive labelling of the isolated oligonucleotides. Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984     

反相高效液相色谱法测定野生与栽培花锚药材及其制剂中的花锚甙和去甲氧基花锚甙

建立了花锚药材及其制剂中两种抗肝炎有效成分花锚甙和去甲氧基花锚甙的反相高效液相色谱测定方法。采用甲醇回流提取进行样品处理,在乙腈 磷酸水溶液为流动相作梯度洗脱、ODS柱、检测波长为254 nm条件下,花锚甙和去甲氧基花锚甙均可达到基线分离。两种成分在0.68～3.40 g/L ,0.36～1.8 g/L 时,其峰面积与浓度成良好的线性关系,加标回收率为95%～105%。该法适用于花锚药材及其制剂的质量分析检验。     

Preparative separation of a terpenoid and alkaloids from Tripterygium wilfordii Hook. f. using high-performance counter-current chromatography. Comparison of various elution and operating strategies

This paper describes how high-performance counter-current chromatography (HPCCC) was used strategically for the separation of Tripterygium wilfordii Hook. f. Due to the complexity of Chinese herbal medicines, the initial ethanol crude extract was fractionated into seven fractions using medium-pressure liquid chromatography (MPLC). One terpenoid (triptolide) and three alkaloids (peritassine A, wilforgine and wilforine) were further separated from one of the MPLC fractions. This fraction (1.25 g) yielded 8 mg of triptolide and 28 mg of peritassines A after one HPCCC column pass and 30 mg of wilforgine and 120 mg of wilforine after a second column pass with respective purities of 97%, 93.6%, 95.0% and 94.4%, which were determined by high-performance liquid chromatography (HPLC). This was a one-step HPCCC separation, using an n-hexane-ethyl acetate-methanol-water (4:5:4:5, v/v) solvent system, where increases in theoretical plates have been sacrificed in favour of increasing throughput. Structures were identified by electrospray ionization mass spectrometry (ESI-MS), (1)H nuclear magnetic resonance ((1)H NMR) and (13)C nuclear magnetic resonance ((13)C NMR). Comparison of three different modes of eluting compounds retained in the liquid stationary phase: elution extrusion; dual mode and simple pump-out showed that simply pumping out the column contents at high flow gave better resolution and was eight times faster than the other two well-utilised methods. Triptolide and peritassines A were isolated for the first time from Tripterygium wilfordii Hook. f.     

Identification of Components of Traditional Chinese Medicine Preparation “Jing-Zhi-Guan-Xin” Troche by Medium Pressure LC and HPLC–DAD–MS

Comprehensive identification of the phytochemical components is one of the key points in the study on traditional Chinese medicine (TCM). In the present study, an approach combining separation and identification of the complex chemical composition in a TCM preparation named “Jing-Zhi-Guan-Xin” (JZGX) troche was developed. Medium pressure liquid chromatography (MPLC) was used to separate JZGX troche into several fractions according to their different polarity. Then, HPLC–DAD–MS was performed to acquire MS and UV spectra of the components within each of the separated fractions. Finally, 64 components were detected, among which, 22 components were identified by comparing their obtained retention times, molecular weights and UV spectra with the available standards and reference data. The results indicate that this approach is beneficial to explore chemical composition of traditional Chinese medicine preparation.     

Separation of nonionic surfactants according to functionality by hydrophilic interaction chromatography and comprehensive two-dimensional liquid chromatography

It is shown, that amphiphilic polymers--such as polysorbates and fatty esters of polyethylene glycol can be separated by comprehensive two-dimensional liquid chromatography using a reversed phase column (under critical conditions for the polyoxyethylene chain) and a HILIC column, which may arranged in different order. The mobile phases in both dimensions can be 93-97 wt% acetone water. As the retention of higher esters on the reversed phase column is very strong, this column should be used as the first dimension. On the HILIC column all fractions elute within a reasonably short time (at a flow rate of 2.5 ml/min within 2 min). With a flow rate of 0.1 ml/min in the first dimension, a full separation can be achieved in 90 min.     

Highly sensitive and accurate profiling of carotenoids by supercritical fluid chromatography coupled with mass spectrometry

We attempted to establish a high‐speed and high‐resolution profiling method for a carotenoid mixture as a highly selective and highly sensitive detection method; the analysis was carried out by supercritical fluid chromatography (SFC) coupled with mass spectrometry (MS). When an octadecyl‐bonded silica (ODS) particle‐packed column was used for separation, seven carotenoids including structural isomers were successfully separated within 15 min. This result indicated not only improved separation but also improved throughput compared to the separation and throughput in RP‐HPLC. The use of a monolithic ODS column resulted in additional improvement in both the resolution and the throughput; the analysis time was reduced to 4 min by increasing the flow rate. Furthermore, carotenoids in biological samples containing the complex matrices were separated effectively by using several monolithic columns whose back pressure was very low. The mass spectrometer allowed us to perform a more sensitive analysis than UV detection; the detection limit of each carotenoid was 50 pg or below. This is the first report of carotenoid analysis carried out by SFC‐MS. The profiling method developed in this study will be a powerful tool for carrying out accurate profiling of biological samples.     

Separation of phospholipid classes by hydrophilic interaction chromatography detected by electrospray ionization mass spectrometry

A new isocratic separation method was developed for separation of phospholipid (PL) classes based on a silica hydrophilic interaction liquid chromatography (HILIC) column with electrospray ionization (ESI) mass spectrometric detection. Although HILIC is typically used for polar compounds, also amphiphilic molecules like phospholipids can be separated very well. Compared to normal-phase (NP) chromatography, which is usually used for PL class separation, HILIC has the advantage to use on-line ESI-MS detection because its eluents are ESI compatible. Furthermore, this HILIC method is isocratic and hence less time consuming than most (gradient) NP HPLC methods. A chromatographic baseline separation of a standard mixture containing phosphatidylglycerol (PG), phosphatidylethanolamine (PE), phosphatidylcholine (PC), sphingomyelin (SM) and lysophosphatidylcholine (LPC) was achieved within a total run time of 17 min using a mobile phase consisting of acetonitrile, methanol and ammonium acetate 10 mM. The new method was subsequently tested on phospholipid fractions of a body fluid (human blood plasma) and a tissue extract (swine brain) whereby it achieved nearly the same baseline separation of the PL classes. The detected classes in both cases were PE, PC, SM and LPC.     

Stationary phase-based two-dimensional chromatography combining both covalent and noncovalent interactions on a single HPLC column

A new type of 2-D separation material was synthesized and studied. The material is suitable for 2-D chromatography utilizing both covalent and noncovalent interactions. The first dimension is boronate affinity chromatography, and the second dimension is RP chromatography (or vice versa). The polymeric media were prepared using p-vinylphenylboronic acid as the functional monomer. This monomer was selected due to the presence of the boronic acid group for the cis-diol/boronate interaction in boronate chromatography. Two crosslinkers were evaluated, namely ethylene glycol dimethacrylate and divinylbenzene. The crosslinker content was varied to maximize the polymer strength and the RP performance of the packed column. Several parameters were evaluated to define the optimum for polymer strength and column performance including crosslinker, porogen, initiator, and column-packing parameters. The polymer-based HPLC columns were successful in separating phenol, catechol, dimethylphthalate, and hydroquinone under RP conditions, and thus can be used as an RP HPLC column. The columns were also successful in separating catechol and adenosine under boronate chromatography conditions, and thus can be used as a boronate affinity column. Moreover, the two types of chromatography can be performed consecutively on the same column during one complete chromatographic run, making it a 2-D chromatography. Under these 2-D conditions, the catechol was separated from a mixture of phenol, catechol, dimethylphthalate, and hydroquinone; the adenosine ribonucleoside was separated from a mixture of adenosine ribonucleoside, adenosine deoxyribonucleoside, and uridine deoxyribonucleoside. This type of single-column 2-D HPLC eliminates the requirement of a complex and expensive multidimensional HPLC instrument and provides increased peak capacity for separation.     

High-performance liquid chromatography of seized drugs at elevated pressure with 1.7 microm hybrid C18 stationary phase columns

High-performance liquid chromatography (HPLC) separation of drugs at elevated pressure with 1.7 microm hybrid C18 stationary phase columns was investigated. This technique, which uses instrumentation engineered to handle the narrow peaks and high back pressures generated by 1.7 microm particle columns, provided significantly better resolution and/or faster analysis than conventional HPLC and capillary electrophoresis (CE). The use of 2mm internal diameter (i.d.) columns of 3-10 cm length has been evaluated for the separation of basic and neutral drugs, drug profiling, and general screening (including acidic drugs). For these applications, compared to conventional HPLC and CE, it provided up to 12x and 3x faster analyses, respectively. Precision was excellent for both isocratic and gradient analyses. For retention time and peak area, RSDs of < or =0.1% were obtainable. Fifteen anabolic steroids and esters were well separated in a 2.5 min gradient. For drug profiling, compared to HPLC and CE, approximately twice as many peaks were resolved. HPLC at elevated pressure is also well suited as a general screening technique. Twenty-four solutes of varying drug classes including narcotic analgesics, stimulants, depressants, hallucinogens, and anabolic steroids were fully separated in a 13.5 min gradient.     

金属硫蛋白异构体及亚型异构体的液相色谱分离与质谱鉴别

建立了金属硫蛋白(MT)异构体及亚型异构体的色谱分离与质谱鉴别方法。将金属硫蛋白混合物通过弱阴离子DEAE Sephadex A-25离子交换柱,结合离线电感耦合等离子体质谱(ICP-MS)对锌诱导金属硫蛋白的两个异构体MT-1和MT-2进行分离和检测;利用Sephadex G-25凝胶排阻色谱柱对得到的两个金属硫蛋白异构体进行脱盐;探索脱盐后的金属硫蛋白异构体在不同色谱条件下的C18反相色谱柱上的保留行为,进而实现各个亚型异构体的分离;通过在线电喷雾质谱检测实现了对金属硫蛋白各个亚型异构体的鉴别。结果表明,通过优化色谱条件,由离子交换色谱及凝胶排阻色谱得到的金属硫蛋白各亚型异构体在酸性条件下均得到了良好的分离,质谱检测结果与前人的文献报道结果一致。该方法可使金属硫蛋白各异构体均达到最佳的分离效果。