Determination of gastrodin,p-hydroxybenzyl alcohol, vanillyl alcohol,p-hydroxylbenzaldehyde and vanillin in tall gastrodia tuber by high-performance liquid chromatography

Summary A high-performance liquid chromatographic method for the separation and determination of gastrodin,p-hydroxybenzyl alcohol, vanillyl alcohol,p-hydroxylbenzaldehyde and vanillin in extract of Chinese herbal medicine tall gastrodia tuber (Chinese name: Tianma) was established. The chromatographic conditions were optimized by means of computer-assisted method development technique. Dry-Lab software was used to model the retention behavior of the compounds as a function of gradient conditions, based on the data from two scouting gradient runs. Under the optimized conditions: column, Kromasil-C18, 5 μm, 15×0.46-cm; solvent A, water; solvent B, methanol; gradient, 5/44/65/65% B at 0/9/12/15 min; flow rate, 1.00 mL min⁻¹; temperature, ambient, the quality of tall gastrodia tubers from different sources and tianma injection were examined.     

老年人的合理用药

老年人由于组织器官的老化和功能减退，影响药物的吸收、分布、代谢和排泄。为确保老年患者的用药安全，应提高老年人的合理用药水平。     

IDENTIFICATION OF PARTIAL MUTATIONAL SITES IN HUMAN MITOCHONDRIAL DNA IN THE CHINESE AND ITS SIGNIFICANCE

A simple method for the identification of mutational sites in human mitochondrial DNA (mtDNA) was described. It was based on the human Cambridge sequence as a relative standard sequence and a single base pair substitution in mtDNA as a unique mutational form. The partial mutational sites can be determined using this method which was characterized by combining the restriction mapping with the analysis for the table of human mtDNA potential mutational sites with rapidity and simplicity. In the meanwhile, six mtDNA mutational sites found in Chinese population were identified by means of this method.     

Assembly of a series of malarial glycosylphosphatidylinositol anchor oligosaccharides

We report an efficient and convergent synthesis of a series of oligosaccharides comprised of the malaria GPI glycan (2a), a promising anti-malaria vaccine candidate currently in preclinical trials and several related oligosaccharide sequences (3-8) that are possible biosynthetic precursors of the malarial GPI. A flexible synthetic strategy is disclosed that relies on a late-stage coupling between oligomannosides of varying length and pseudo-disaccharide glycosyl acceptor 11 to readily access various malarial GPI structures. Phosphorylation was accomplished by mild and efficient H-phosphonate chemistry before the final deprotection was carried out by using sodium in ammonia. The direct connection of a thiol group via a phosphate diester linkage to the inositol moiety provides a handle for easy conjugation of the GPI glycan to carrier proteins, immobilization on carbohydrate microarrays and photo-affinity labels identification. These synthetic oligosaccharides will serve as molecular probes.     

Total Synthesis of Sialylated Glycans Related to Avian and Human Influenza Virus Infection

Human and avian influenza type A viruses bind sialylated pentasaccharides. Herein, the total synthesis of four of these glycans is reported. Efficient sialylations relied on two N‐Troc‐protected (Troc=2,2,2‐trichloroethoxycarbonyl) sialic acid building blocks. The first, a thiophenyl glycoside, readily produced the sialyl‐α(2‐6)galactose disaccharide. Combination of the second building block, a novel glycosyl phosphite, and a benzylidene‐protected galactoside produced the best results for the formation of the sialyl‐α(2‐3)galactose. Two common trisaccharides were assembled by the introduction of glucose, galactose, and glucosamine building blocks followed by selective deprotection. Two sets of pentasaccharides were obtained by the union of two sialylgalactose N‐phenyl trifluoroacetimidate building blocks with the two trisaccharides above. Global deprotection furnished the desired pentasaccharides. The products of these total syntheses are currently employed on the surface of carbohydrate microarrays to detect and type different strains of the influenza virus.     

SARS-CoV protease inhibitors design using virtual screening method from natural products libraries

Two natural products databases, the marine natural products database (MNPD) and the traditional Chinese medicines database (TCMD), were used to find novel structures of potent SARS-CoV protease inhibitors through virtual screening. Before the procedure, the databases were filtered by Lipinski's ROF and Xu's extension rules. The results were analyzed by statistic methods to eliminate the bias in target-based database screening toward higher molecular weight compounds for enhancing the hit rate. Eighteen lead compounds were recommended by the screening procedure. They were useful for experimental scientists in prioritizing drug candidates and studying the interaction mechanism. The binding mechanism was also analyzed between the best screening compound and the SARS protein.     

碘酸钾存在下极谱催化波法测定陈皮甙

基于陈皮甙在ＫＩＯ３存在下产生的极谱催化波，拟定了测定陈皮甙的新方法。在 ０．５５ ｍｏｌ／Ｌ ＨＡｃ－０．０１ｍｏｌ／Ｌ　ＮａＡｃ（ｐＨ ４．００±０．０５）－１．０×１０～（－３）ｍｏｌ／Ｌ ＫＩＯ３缓冲溶液中，陈皮甙催化波的峰电位为－１．３５ Ｖ（ｖｓ，ＳＣＥ），它的一阶导数峰峰电流与陈皮甙浓度在２．６ × １０～（－７）～２．６ × １０～（－６）ｍｏｌ／Ｌ范围内呈线性关系（ｒ＝０．９９７０，ｎ＝６）。本方法比现有的电化学方法灵敏度高一个数量级。可用于直接测定中草药贯众水提液中陈皮甙含量。     

One-pot synthesis of sialo-containing glycosyl amino acids by use of an N-trichloroethoxycarbonyl-beta-thiophenyl sialoside

We describe an efficient synthesis of 2,6- and 2,3-sialyl T antigens linked to serine in a one-pot glycosylation. We first investigated the glycosidation of thiosialosides by varying the N-protecting group. Modification of the C-5 amino group of beta-thiosialosides into the N-9-fluorenylmethoxycarbonyl, N-2,2,2-trichloroethoxycarbonyl (N-Troc), and N-trichloroacetyl derivatives enhanced the reactivity of these compounds towards glycosidation. Addition of a minimum amount of 3 A molecular sieves was also effective in improving the yield of alpha-linked sialosides. Next, we conducted one-pot syntheses of the glycosyl amino acids by using the N-Troc sialyl donor. The N-Troc derivative can be converted into the N-acetyl derivative without racemization of the amino acids. Branched-type one-pot glycosylation, initiated by regioselective glycosylation of the 3,6-dihydroxy galactoside with the N-Troc-beta-thiophenyl sialoside, provided the protected 2,6-sialyl T antigen in good yield. Linear-type one-pot glycosylation, initiated by chemoselective glycosylation of galactosyl fluoride with the N-Troc-beta-thiophenyl sialoside, afforded the protected 2,3-sialyl T antigen in excellent yield. Both protected glycosyl amino acids were converted into the fully deprotected 2,6- and 2,3-sialyl T antigens linked to serine in good yields.     

GC/MS法分析油松节挥发油化学成分

用气相色谱-质谱法对山东昆嵛山产油松节挥发油进行化学成分的分析。采用水蒸气蒸馏法从油松节中提取挥发油。采用不同类型的毛细管柱进行分析，找出最佳分析条件，用归一化法测定其含量，并用气相色谱-质谱法对化学成分进行鉴定。共鉴定了48个成分，占挥发油总成分的84％以上。结果表明，此方法稳定可靠，重现性好，适用于中药挥发油的化学成分分析。     

A study for quality evaluation of Taxilli Herba from different hosts based on fingerprint-activity relationship modeling and multivariate statistical analysis

In this study, a fingerprint-activity relationship modeling between chemical fingerprints and antirheumatic activity was established, and multivariate statistical analysis was used to evaluate the quality of Taxilli Herba (TH) from different hosts. Characteristic fingerprints of 20 batches of TH samples were generated by high-performance liquid chromatography coupled with triple quadrupole-time of flight tandem mass spectrometry (HPLC-Triple TOF-MS/MS), and the similarity analysis was calculated based on thirteen common characteristic peaks by hierarchical clustering analysis (HCA). Subsequently, nine efficacy markers were discovered by combining fingerprints and antirheumatic activity through grey correlation analysis (GCA) and bivariate correlation analysis (BCA). Meanwhile, the content of 5 constituents in 9 markers was determined by high-performance liquid chromatography coupled with triple quadrupole-linear ion trap tandem mass spectrometry (HPLC-QTRAP-MS/MS). The comprehensive quality of TH was assessed using multivariate statistical analysis, including principal components analysis (PCA) and technique for order preference by similarity to ideal solution (TOPSIS). The results showed that a high dose of TH extract could markedly ameliorate arthritis damage compared to other doses, with flavonoids playing an important role in the antirheumatic activity. The comprehensive quality of samples from Morus alba L. (SS) was superior to those from Liquidambar formosana Hance (FXS). The present study will demonstrate the markers associated with efficacy, and provide an applicable strategy for more comprehensive quality control and evaluation of TH.