胶束液相色谱

胶束液相色谱(micellar liquid chromatography),又叫假相液相色谱(pseudophase liquid chromatography),使用高于临界胶束浓度(CMC)的表面活性剂溶液作流动相,代替液相色谱传统的水-有机物流动相。胶束流动相不仅具有毒性小(避免使用甲醇、乙腈)、消     

间接液相色谱电化学法测定酯类化合物

本文用间接液相色谱电化学的方法对非电活性的酯类混合物甲酸甲酯、甲酸乙酯、乙酸甲酯和乙酸乙酯进行了分离和测定,其线性范围分别是3.2×10~(-9)～4.4×10~(-8)mol、2.4×10~(-9)～2.8×10~(-8)mol、2.0×10~(-9)～4.0×10~(-8)mol和2.2×10~(-9)～2.4×10~(-8)mol。对甲酸甲酯8次平行测定的相对标准偏差为0.89％。     

制备液相色谱结合液相色谱-气相色谱联用技术高灵敏检测化妆品中的芳烃矿物油

矿物油是化妆品的重要原料,其主要成分是烷烃矿物油(MOSH),但其中残留的芳烃矿物油(MOAH)会危害人体健康。然而,高比例的MOSH使得化妆品中微量MOAH的分析非常困难,即使采用液相色谱-气相色谱联用技术(LC-GC)也难以准确测定。本研究采用制备液相色谱(Prep-LC)结合LC-GC建立了化妆品中MOAH的高灵敏检测方法。首先采用乙醇和正己烷提取,然后加水实现相分离,得到矿物油提取液;再经过预净化,注入Prep-LC分离。Prep-LC采用纯硅胶柱(250 mm×10 mm, 5μm),洗脱溶剂为正己烷-二氯甲烷二元体系,通过梯度洗脱,可分离去除2 mg以上的MOSH,制备得到高纯度的MOAH组分;经LC-GC和全二维气相色谱-飞行时间质谱(GC×GC-TOFMS)验证,Prep-LC制备的MOAH不含MOSH干扰物。最后,将收集的MOAH浓缩并注入LC-GC进行测定。方法学考察结果表明,本方法的定量限为10 mg/kg,回收率为82.0%～100.8%, RSD为3.6%～7.3%。采用本方法对市售15个口红和唇膏样品进行检测,其中4个样本检出MOAH,含量为204～1460...     

填充毛细管液相色谱-高温毛细管气相色谱在线联用分析重油

重油的组成分析一直是个难题,它的沸点高,族组分种类多,各族内组分的异构体又极为繁多.最好的分析方法是用高效液相色谱(HPLC)做族分离,馏分收集后再用CGC分析.但HPLC的族馏分体积比CGC进样量大100倍.本文采用填充毛细管液相色谱(μHPLC)与高温毛细管气相色谱(HTGC)在线联用技术[1]分析重油.正相μHPLC将样品按族分离,μHPLC的柱效高,族分离能力强,而小的馏分体积(<100μL)可避免GC分流进样.在一次LC进样后,多位储存型联用接口将分离后的各族组分切割、存储并分别无损失转入HTGC分析,利用FID对高于C10的有机物的响应值相…     

胶束反相高效液相色谱最佳化研究

本文介绍以YWG-C_(18)为固定相,十二烷基硫酸钠(SDS)胶束溶液为移动相,探讨了SDS浓度和柱温对胶束反相高效液相色谱分离最佳化的影响。测定了胶束体系中苯胺的热力学函数ΔH~0值及SDS的临界胶束浓度(C.M.C.),还讨论了非极性和极性溶质的保留机理。     

卡尔曼滤波在高效液相色谱中的应用

前言 近十年来,从实验数据中得到更多的信息已经成为分析化学中的一个重要研究领域。数字滤波已在分析化学的很多方面得到应用。所谓滤波,就是把信号的一个成分与另一些成分分开,进行滤波可减少噪声的影响,并使含有有用信息的信号(如峰形或峰高)变形最小。卡尔曼滤波(Kalman filter)是一种递推式算法和适用于小型     

高效液相色谱质谱质谱法分析人参皂甙

 以反相高效液相色谱法分离了 9种人参皂甙。操作条件为乙腈 水梯度洗脱 ,二极管阵列检测器检测并在2 0 2nm下提取色谱图。利用三级四极杆质谱研究了 9种人参皂甙的一级质谱 (主要给出相对分子质量信息 )和二级质谱 (提供碎片结构信息 )。通过它们质谱图的差异对其进行了鉴别 ,并将方法用于实际样品中的 9种人参皂甙的定性。     

微柱液相色谱的研究进展

介绍了微柱液相色谱（μ-LC）。从理论上简单讨论了μ-LC的柱特性、色谱洗脱效应和柱外效应等一系列问题,综述了μ-LC的柱技术的最新进展,讨论了μ-LC对仪器和附件的要求,特别是微流量输液和检测技术,还探讨了μ-LC与多维色谱、质谱等技术的联用。     

反相高效液相色谱法测定山荷叶中木脂素含量

山荷叶(Diphylleia sinensis Li)系小蘖科山荷叶属植物,其根茎民间主要用于痈疖肿毒、跌打、蛇咬伤等。药理实验证明其主要成分鬼臼、毒素类木脂素具有抗肿瘤、抗病毒、抑制细胞中期有丝分裂等活性。由鬼臼毒素作为前体合成了一系列抗癌     

生物工程下游处理中的液相色谱

生物工程的最终目的是要制造出能为人类所利用的产品。这种产品将主要是蛋白质或多肽,这种产品往往应具有极高的纯度,特别是当把它们做为医药制品时。因此目前普遍认为,在生物工程的研究成果转化成为有商品价值的产品的过程中,其下游处理(即对原核或真核细胞产物的分离纯化过程)的花费将在全部生产成本中占有最主要的份额。     

人工蚕蛹虫草和冬虫夏草水溶性成分的相对归属分析

为对相近中药的化学指纹图谱进行比较研究,充分利用联用色谱所得的光谱、色谱信息与光谱相关色谱方法,分析了蚕蛹虫草和冬虫夏草的水溶性成分的异同,实现了蚕蛹虫草和冬虫夏草水溶性成分化学指纹图谱中相应化学组分的归属分析。其中,蚕蛹虫草和冬虫夏草有5个共有组分,分别有4个和6个相异组分。实验表明：该方法可对复杂中药成分及其指纹图谱进行快速比较分析。     

均匀设计在蚕蛹虫草和冬虫夏草活性成分分析中的应用

采用均匀实验设计方法快速找到蚕蛹虫草活性成分的高效液相色谱最优分离条件;将该优化条件用于蚕蛹虫草和冬虫夏草的水溶性成分的分离取得满意结果,并对部分组分进行了定性定量分析;均匀实验设计方法可较快找到复杂未知或半未知体系的色谱分离条件。     

Analysis of the Nucleoside Content of Cordyceps sinensis Using the Stepwise Gradient Elution Technique of Thin-Layer Chromatography

Nucleoside is the main class of active components in Cordyceps sinensis. Thin-layer chromatography (TLC) is one of the most commonly used methods in pharmacopoeias for analyzing chemical components of herbal medicine. Since the isocratic elution method cannot be applied successfully in TLC analysis for separating all the nucleoside components, the stepwise gradient elution has been developed in this work to separate eight nucleoside standards with success. In this way, quantitative analyses of the samples of Cordyceps sinensis were achieved via the proposed TLC procedure coupled with the scanning densitometric techniques of CAMAG and TLCQA methods for qualitative and quantitative analysis.     

HELP法在中草药分析中的应用研究-冬虫夏草的化学成分测定

基于直观推导式演进特征投影（ＨＥＬＰ）法,对冬虫夏草子座和虫体分别进行了多组分同时定性定量测定．结果表明,ＨＥＬＰ法能减少样本提取分离的步骤,降低色谱分离条件的要求,提高检测准确度．联用色谱检测与化学计量学解析法相结合将为复杂中草药分析提供一种全新手段     

Simple HPLC-UV determination of nucleosides and its application to the authentication of Cordyceps and its allies

A simple HPLC-UV method combined with a simple extraction procedure of nucleosides (adenosine, cordycepin, 2'-deoxyadenosine, guanosine and uridine) was developed and applied to the authentication of Cordyceps and its allies. The separation was performed on a C(18) column by isocratic elution with acetonitrile-water, and UV detection at 260 nm. The amounts of adenosine, cordycepin, 2'-deoxyadenosine, guanosine and uridine in Cordyceps were 0.28-14.15, 0.006-6.36, 0.01-0.14, 0.68-14.79 and 0.19-20.29 mg/g, respectively. Among the nucleosides studied, cordycepin was characteristically included in Cordyceps militaris (L.) Link. (CM), which is one of key Cordyceps allies, and might be a good marker for authenticating CM. The ratio of nucleosides to adenosine contents in Cordyceps seemed to be a useful marker for authentication and quality control of Cordyceps.     

Analysis of the Water Soluble Constituents of Cordyceps Sinensis With Heuristic Evolving Latent Projections

ABSTRACT

A chemometric technique, heuristic evolving latent projection (HELP), was applied to analyze the data obtained from high performance liquid chromatography coupled with the diode array detection (HPLC-DAD) for a traditional Chinese medicinal herb, Cordyceps sinensis. Based on this method, the water soluble components, nucleosides in Cordyceps sinensis were identified. Ten and eleven volatile components were identified from the fungal and larvae parts of Cordyceps sinensis sample, respectively. As compared with the conventional method, HELP was found to be suitable for quantitative analysis of complex real systems such as Chinese medicinal products.     

碳纳米管修饰电极测定冬虫夏草有效成分含量

以多壁碳纳米管修饰金电极为工作电极测定了冬虫夏草胶囊有效成分的含量。结果表明,在pH值为7.0的缓冲溶液中,测得其极化电流与腺嘌呤核苷在浓度为1.0×10-4～1.0×10-8mol/L范围内呈良好的线性关系(R2=0.9947),检出限为1.0×10-9mol/L。所测的5批样品的平均回收率为101.5%,相对标准偏差RSD为1.5%。方法灵敏度高、简单、快速、重现性好、干扰小,而且节能、环保,无污染物排放。     

Extraction, Purification and Anti-tumor Activity of Polysaccharide from Mycelium of Mutant Cordyceps Militaris

A water-soluble polysaccharide(named MCMP) was isolated from the mycelium with high yield mutation Cordyceps militaris by hot-water extraction, deproteinization by sevage, alcohol precipitation, anion-exchange and gel filtration chromatography CL-6B. The polysaccharide contained mannose, rhamnose, galactose and glucose in a molar ratio of 59.36:1:8.31:39.50, of which the average molecular weight is 8100. In our research, Hep-G2 cells, Hela cells and mesangial cells were chosen to determine the anti-tumor activity of the polysaccharide. The results of MTT assay show that polysaccharides of the mutant strain presented inhibitory activity on the cells proliferation after 48 h incubation.     

Isochromanes from Aspergillus fumigatus,an endophytic fungus from Cordyceps sinensis

Four previously undescribed isochromanes were isolated from the fermentation broth of an endophytic fungus Aspergillus fumigatus, which was obtained from the fruiting body of Cordyceps sinensis. Their structures were elucidated through extensive spectroscopic analyses. One racemic isochromane was further purified by chiral HPLC to yield a pair of enantiomers and their absolute configurations were determined by quantum chemical ECD calculations. These isolated compounds were evaluated for cytotoxicity against two cell lines (MV4-11 and MDA-ME-231) and the result showed that compounds 1a and 2 exhibited moderate growth inhibition against MV4-11 cell line.     

Quality evaluation of Cordyceps through simultaneous determination of eleven nucleosides and bases by RP-HPLC

A new RP-HPLC method has been developed for the simultaneous determination of 11 nucleosides and bases, including adenosine, cordycepin, cytidine, guanosine, inosine, thymidine, uridine, cytosine, guanine, thymine, and uracil in Cordyceps. Determination was achieved on a Zorbax 300SB C18 analytical column (4.6 x 250 mm id, 5 mm) using gradient elution with diode-array detection. All calibration curves showed good linearity (r2 > 0.9995) within the test ranges. The developed method was simple, rapid, and accurate, and showed good reproducibility for the quantification of 11 nucleosides and bases in natural and cultured Cordyceps with both intra- and inter-day variations of less than 1.8%. Furthermore, hierarchical clustering analysis based on the typical peaks of adenosine, cordycepin, and inosine in HPLC profiles from the 11 tested samples showed that natural and cultured Cordyceps were in different clusters, which could provide a means of discriminating between Cordyceps of different origins. Thus, adenosine, cordycepin, and inosine could be used as markers for quality control of Cordyceps.