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总结了手性逆流色谱的5个特点,系统地介绍了逆流色谱的手性分离以及高速逆流色谱手性分离中氨基酸衍生物、环糊精衍生物、手性有机酸、多糖衍生物、牛血清白蛋白等手性选择剂的应用。 相似文献
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中药挥发油成分复杂,一维色谱分离由于有限的峰容量难以完全分离中药挥发油成分,全二维气相色谱为分离挥发油成分提供了有力的方法,然而气相色谱一般无法用于天然活性成分的筛选。为建立挥发油成分全二维色谱分析新方法,研究建立以液相色谱为基础的全二维色谱分离分析方法。本文主要研究全二维逆流色谱-液相色谱分离莪术油成分的方法,并探讨两种色谱技术之间的正交性,为活性成分筛选提供新的技术支持。通过优化离线全二维逆流色谱-液相色谱分离方法,对全二维色谱峰容量、正交性和空间覆盖率进行度量。优化液相色谱分析条件并筛选逆流色谱分离两相溶剂体系,通过比色法筛选了逆流色谱两相溶剂体系并采用下相为流动相进行梯度洗脱。在290~375 min采用推挤洗脱,莪术油在第一维逆流色谱分离中达到了良好的分离。第二维反相高效液相色谱的流动相组成为乙腈(A)和水(B)。梯度洗脱程序为0~10 min, 50%A~65%A; 10~14 min, 65%A; 14~21 min, 65%A~85%A; 21~25 min, 85%A~95%A; 25~30 min, 95%A~55%A; 30~40 min, 55%A。在上述条件下... 相似文献
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该文建立了大孔树脂-高速逆流色谱分离薇甘菊中黄酮类物质的方法。分离条件为:采用大孔树脂AB-8,洗脱液为50%(v/v)乙醇水溶液,高速逆流色谱溶剂体系为正丁醇-乙酸-水(4:1:5,v/v)。从薇甘菊中分离到4种黄酮类物质:槲皮素-3-O-芸香糖苷(纯度90.2%)、山奈酚-3-O-芸香糖苷(纯度98.55%)、木犀草苷(纯度98.33%)和紫云英苷(纯度99.23%)。建立的大孔树脂-高速逆流色谱方法简单、高效,可扩展应用于从其他植物中分离黄酮类物质。 相似文献
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《Biomedical chromatography : BMC》2017,31(11)
Characterization of the glycans of glycoproteins is essential for the development and production of biologics. Numerous methods are available for analyzing the glycans of glycoproteins directly and labeled glycans. Nevertheless, glycopeptides are difficult to resolve because of their exceptional complexity and the microheterogeneity of glycans. These properties represent technical challenges to efforts to insure the accurate characterization of biopharmaceuticals to comply with regulatory requirements. Therefore, we investigated the retention behavior of peptides and glycopeptides in hydrophilic interaction chromatography‐mode HPLC in the presence of ion‐pairing reagents. Anionic ion‐pairing reagents decreased the retention times of glycopeptides and improved resolution in the presence of higher concentrations or hydrophobicities of ion‐pairing reagent. Anionic ion‐pairing reagents increased retention times of larger glycans because of their increased hydrophilicity. In contrast, in the presence of cationic ion‐pairing reagents, the retention times of glycopeptides with greater numbers of sialic acid residues decreased. It is appropriate to add an anionic ion‐pairing reagent to the mobile phase for good separation of glycopeptides. The collision cross‐sectional area values of glycopeptides determined using electrospray ionization‐ion mobility spectrometry‐mass spectrometry correlated with retention times. These findings support the implementation of hydrophilic interaction chromatography‐mode HPLC to improve the characterization of glycosylated biopharmaceuticals. 相似文献
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Summary The use of over-pressurized thin-layer chromatography in ion pair system using acidic type pairing reagent has been studied.
The most important aspect when reversed phase ion-pair TLC system is used to apply a suitable procedure for pre-treatment
of the sorbents. Because of the acidic type of ion pair reagents cannot be bounded to the surface of the layer by immersion
or pre-development with the reagent solution, double coating technique was used for the pre-treatment, the plate was firstly
immersed in an ethanolic solution of cetrimide, then the immersion has been repeated by an ethanolic solution of acidic ion
pair reagent. The necessary coating of the sorbents can be achieved by this technique.
To find the optimal conditions for reversed phase ion pair TLC separation of organic amines, 10-camphor sulfonic acid as reagent,
different aliphatic, aromatic amines and diamines and heterocyclic nitrogen compounds, respectively as model compounds were
selected. The dependence of the selectivity and efficiency of the separation on the sorbents, on the concentrations of reagents
(cetrimide and camphor sulfonic acid) applied for both immersion and in the eluent were investigated in detail.
Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984 相似文献
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Dash K Thangavel S Rao SV Chandrasekaran K Chaurasia SC Arunachalam J 《Journal of chromatography. A》2004,1036(2):223-227
Trace levels of phosphorus in purified quartz are determined by ion chromatography. In situ reagent purification, matrix digestion and oxidation of phosphorus to orthophosphate ion are carried out simultaneously in a vapour phase digestion (VPD) assembly using a mixture of HF, HNO3 and H2O2. A drastic reduction (475 times) in phosphate blank from reagents (HF/H2O2) was achieved in the VPD through in situ purification of the reagent. The residues remaining after volatilisation (solvent/matrix), mostly consisting of insoluble phosphate/fluoride salts of divalent and trivalent cations, were solubilised by ion-exchange dissolution. Phosphate was analysed on the IonPac AS17 column with suppressed conductivity detection. The results of the ion chromatography (IC) method were compared with a spectrophotometric method. Accuracy was evaluated by analysing a certified reference material (silicon, NIST 57a). The method detection limit was 0.05 microg g(-1). 相似文献
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The principle of sequential injection (SI) was exploited to develop a fully automated pre-column derivatization procedure combined on-line to liquid chromatography (LC). Using SI-LC derivatization 14 amino acids were determined fluorimetrically in pharmaceuticals with o-phthaldialdehyde (OPA) as the derivatization reagent. The SI system was used for the handling of samples and reagents, on-line mixing and introduction to the LC injection system. Chemical (pH and reagents concentrations) and instrumental variables (sample and reagent volumes, reaction time and flow rate) were optimized to attain the highest reaction yield and detector signal. Reversed phase chromatographic resolution of 14 amino acids was achieved within 35 min using gradient elution. The automated operation of the coupled SI-LC system resulted in very satisfactory performance. The method was applied for the simultaneous determination of amino acids in pharmaceutical formulations. 相似文献
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本文研究了具有特殊结构的氢硼酸金属有机络合物的反相色谱及机理。在MicropakC_(18)柱上,加入含离子试剂的甲醇-水作为流动相,通过用电导法测定流动相电性能,Break-through法测定离子试剂在固定相上的吸附量及制备色谱法研究各流分组成,认为此类化合物的保留机理为动态离子交换过程。 相似文献
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《液相色谱法及相关技术杂志》2012,35(14):3161-3172
Abstract New derivatization methods using chiral ferrocene reagents have been developed for the optical resolution of carboxylic acids by high-performance liquid chromatography with electrochemical detection. Two chiral derivatization reagents, 1-ferrocenylethylamine and 1-ferrocenylpropylamine, were readily prepared from acetylferrocene and propionylferrocene in two steps, respectively. Condensation of carboxylic acids with the chiral reagent was effected in the presence of water-soluble carbodiimide and 1-hydroxybenzotriazole. The diastereomeric amides formed from N-acetylamino acid and α-arylpropionic acid enantiomers were efficiently resolved by reversed-phase chromatography and showed the satisfactory sensitivity at +0.45 V vs. an Ag/AgCl reference electrode with a detection limit of 0.5 pmole (S/N=5). 相似文献
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A LC-MS/MS method using a LC column packed with sub-2 micron particles and elevated column temperatures was validated for the quantitation of SCH 503034 diastereomers (SCH 534128 and SCH 534129) in human plasma. The method was validated over the concentration range of 2.5 to 1250 ng/mL. Inter-assay precision, based on percent relative deviation for n = 18 replicate quality controls, was 4.5% for SCH 534128 and 4.9% for SCH 534129. Inter-assay accuracy based on n = 18 replicate quality controls was +/- 7.8% for both SCH 534128 and SCH 534129. The method involved the novel application of ion pairing reagents to increase the stereoselectivity of the separation. Temperature, types of ion pairing reagent, and concentration of ion pairing reagent were all found to play significant roles in the resolution of the SCH 534128 and SCH 534129 diastereomers on a LC column packed with sub-2 micron particles. Specifically, a sensitivity increase of five-fold was demonstrated by increasing the column temperature. Without sacrificing resolution, the run time was significantly shortened when the column temperature was elevated to 100 degrees C. 相似文献
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Recently, we reported on a phenomenon in which multiply charged protein cations produced by electrospray ionization could be reduced to lower and narrower charge state distributions when admixed with reducing reagents 1,4-benzoquinone or quinhydrone. Circular dichroism spectra of the proteins indicated that secondary and tertiary structural changes upon addition of these reducing reagents were negligible, thus eliminating conformational effects as playing a role in the charge reduction mechanism. Furthermore, the extent of charge state reduction did not correspond with gas-phase basicities of the redox reagents, suggesting that solution-phase, and not gas-phase, behavior dominates the observed charge state reduction. The relatively low resolution of the triple quadrupole employed did not make it possible to distinguish isotopic distributions of the multiply charged cations in order to determine whether the observed phenomenon was the result of proton-transfer reactions between the multiply charged cations and the reducing reagent or because of electron transfer from the reducing reagent to the protein cations. Here, high-resolution ESI-Fourier transform ion cyclotron resonance mass spectrometry of several peptide amides in the presence of a redox reagent show isotopic distributions that are consistent only with the proton-transfer mechanism. 相似文献
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Blackcurrant is considered as a natural high-value food raw material and possesses a variety of therapeutic properties. The health benefits of blackcurrant have generally been credited to its high anthocyanin content; however, the therapeutic properties of other minor flavonoids constituents have not yet been investigated due the difficulties related to their isolation. Multiple steps of high-performance counter-current chromatography in combination with ESI tandem mass spectrometry (MS(n)) were successfully used for the preparative isolation of flavonols from blackcurrant extract, to study their electrospray ionization mass spectrometry fragmentation behavior. Seven flavonols, namely myricetin-3-O-rutinoside (145.5 mg), myricetin-3-O-hexoside (79.7 mg), myricetin-3-O-(6″-malonyl)-glucoside (17.4 mg), kaempferol-3-O-glucoside (20.5 mg), quercetin-3-O-rutinoside (55.1 mg), quercetin-3-O-hexoside (25.8 mg), and myricetin (129.1 mg) have been successfully isolated and their multistage MS(n) data were used for detailed structure characterization. The results of these experiments demonstrated that high-performance counter-current chromatography along with ESI-MS(n) is a sensitive, selective, and effective technology for isolation and characterization of minor constituents from a complex mixture. 相似文献