Xiuli Zhang

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Name: 张秀莉; Zhang, XiuLi

Organization: Chinese Academy of Sciences , China

Department: Dalian Institute of Chemical Physics

Title: (PhD)

Chemicals
References

Discovery of 2H-Chromen-2-one Derivatives as G Protein-Coupled Receptor-35 Agonists

Co-reporter:Lai Wei, Jixia Wang, Xiuli Zhang, Ping Wang, Yaopeng Zhao, Jiaqi Li, Tao Hou, Lala Qu, Liying Shi, Xinmiao LiangYe Fang

Journal of Medicinal Chemistry 2017 Volume 60(Issue 1) pp:

Publication Date(Web):December 15, 2016

DOI:10.1021/acs.jmedchem.6b01431

A family of 2H-chromen-2-one derivatives were identified as G protein-coupled receptor-35 (GPR35) agonists using dynamic mass redistribution assays in HT-29 cells. The compounds with 1H-tetrazol-5-yl in 3-substituted position displayed higher potency than the corresponding carboxyl analogs, and the hydroxyl group in the 7-position also played an important role in GPR35 agonistic activity. 6-Bromo-7-hydroxy-8-nitro-3-(1H-tetrazol-5-yl)-2H-chromen-2-one (50) was found to be the most potent GPR35 agonist with an EC50 of 5.8 nM. Calculating the physicochemical properties of compounds with moderate to high potency suggested that compounds 30, 50, and 51 showed good druggability. This study provides a novel series of GPR35 agonists, and compound 50 may be a powerful tool to study GPR35.

Preparative separation of a challenging anthocyanin from Lycium ruthenicum Murr. by two-dimensional reversed-phase liquid chromatography/hydrophilic interaction chromatography

Co-reporter:Hongli Jin, Jianqiang Zhao, Weijia Zhou, Aijin Shen, Fan Yang, Yanfang Liu, Zhimou Guo, Xiuli Zhang, Yanduo Tao, Xiaojun Peng and Xinmiao Liang

RSC Advances 2015 vol. 5(Issue 76) pp:62134-62141

Publication Date(Web):14 Jul 2015

DOI:10.1039/C5RA08713A

The preparative separation of anthocyanins by HPLC often suffers from insufficient separation selectivity. In this work, a two-dimensional liquid (LC-LC) method was established to efficiently purify a challenging anthocyanin in Lycium ruthenicum Murray. Reversed phase liquid chromatography (RPLC) was used in the first-dimension preparation to fractionate the sample for its high separation efficiency. After the optimization of second-dimension methods, hydrophilic interaction chromatography (HILIC) was applied to further isolate the anthocyanin for the good orthogonality to RPLC. To improve HILIC separation for anthocyanins, stationary phases and mobile phases were investigated systematically. A satisfactory result was obtained on a zwitterionic Click XIon column with 1% phosphoric acid as an acidic additive. Using the above method, the anthocyanin and three new alkaloids were isolated from L. ruthenicum for the first time. This RPLC/HILIC method solved the coelution problem of anthocyanin and basic non-anthocyanins in one-dimensional HPLC, benefiting from the significantly improved separation resolution.

Discovery of new targets of phenolic acids in danshen using a label-free cell phenotypic assay

Co-reporter:Jixia Wang, Tao Hou, Lai Wei, Liying Shi, Jian He, Nan Zhou, Guangwei Sun, Xiuli Zhang and Xinmiao Liang

RSC Advances 2015 vol. 5(Issue 33) pp:25768-25776

Publication Date(Web):26 Feb 2015

DOI:10.1039/C4RA16102E

Traditional Chinese medicines (TCMs) have been used in the clinic for thousands of years. Their reliable therapeutic efficacies are closely related to their multi-target mechanisms of action (MOAs). Discovery of these targets is important for understanding their clinical features. Danshen is the dried root of Salvia miltiorrhiza, a Traditional Chinese Medicine (TCM) used for the treatment of cardiovascular and cerebrovascular diseases. Although its clinical features are well recognized, the targets of its active constituents are poorly understood. Here, a label-free cell phenotypic assay was used to investigate the potential targets of the phenolic acids in danshen. Pharmacological profiling of 10 known phenolic acids in danshen using HT-29 and A431 cells revealed that lithospermic acid, salvianolic acid A, salvianolic acid B, salvianolic acid C and danshensu all displayed agonistic activity towards GPR35; however, salvianolic acid A and salvianolic acid C at high doses were also active in altering intracellular Ca2+ via another unknown target. Since GPR35 has been implicated in inflammation and cardiovascular diseases, the discovery of GPR35 as one target of the phenolic acids in danshen was useful for elucidating their mechanisms of action in the treatment of these diseases. This study also highlights the potential of label-free cell phenotypic assays for discovering multiple targets of TCMs.

Characterization of anthocyanins in wild Lycium ruthenicum Murray by HPLC-DAD/QTOF-MS/MS

Co-reporter:Hongli Jin, Yanfang Liu, Fan Yang, Jixia Wang, Dongmei Fu, Xiuli Zhang, Xiaojun Peng and Xinmiao Liang

Analytical Methods 2015 vol. 7(Issue 12) pp:4947-4956

Publication Date(Web):06 May 2015

DOI:10.1039/C5AY00612K

L. ruthenicum, which grows mainly in the salinized desert of the Qinghai-Tibet plateau, contains abundant anthocyanins. To date, information on its anthocyanin composition is still limited. In this work, the systematic characterization of anthocyanins in L. ruthenicum was carried out by HPLC-DAD/QTOF-MS/MS. Six mono-acylated anthocyanins isolated from L. ruthenicum were analyzed by ESI-QTOF-MS/MS, and their fragmentation behaviors were investigated and summarized. Different anthocyanins could be identified through the characteristic product ions and their relative intensities. In addition, various rules were applied to cope with the difficulty of rapidly differentiating cis–trans anthocyanin isomers. A spectral rule was first proposed from the UV/Vis spectra of two pairs of cis–trans anthocyanin isomers. This rule provided important information for the identification of the isomers. Based on these rules, sixteen anthocyanins in L. ruthenicum were tentatively characterized, and seven of them were reported in this plant for the first time. In order to validate the method, an anthocyanin was isolated from L. ruthenicum and identified by NMR and MS.

A novel method for characterization and comparison of reversed-phase column selectivity

Co-reporter:Jixia Wang, Chaoran Wang, Zhimou Guo, Xuefang Dong, Yuansheng Xiao, Xingya Xue, Xiuli Zhang, Xinmiao Liang

Journal of Chromatography A 2014 Volume 1361() pp:153-161

Publication Date(Web):26 September 2014

DOI:10.1016/j.chroma.2014.08.005

•A method for characterizing and comparing column selectivity in RPLC was developed.•LSERs equations at different percentages of organic modifier were obtained.•LSERs equations at pure water were used to characterize column selectivity.•Angles and a spider diagram were helpful for selecting proper columns.•Two columns with best selectivity were used to develop a two dimensional system.Characterization of reverse-phase column selectivity is helpful for chromatographers to select an optimal column. A novel method, based on linear solvation energy relationships (LSERs) combined with fundamental retention equations, was developed to characterize and compare reversed-phase column selectivity. The retention times of 25 elaborately selected solutes on 12 reversed-phase columns were determined in three linear gradient elutions. Using these retention times, fundamental retention equations were acquired by a complex sample analysis software system (CSASS). When 0%, 10%, 20%, 30%, 40% and 50% acetonitrile were introduced into the fundamental retention equations, the corresponding retention factors were predicted and used to obtain LSER equations by multiple linear regression. In the gradient elution, the retention times of solutes could be accurately determined and the excessively long or short analysis time could be avoided. As the retention factor (ln kw) at a hypothetical 0% organic modifier closely reflected properties of columns, coefficients of LSERs equations obtained based on ln kw were employed to discuss the properties of different stationary phases. An angle and a spider diagram based on solvation energy vectors were used to compare selectivity differences between stationary phases, which provided a visual means for users to select appropriate columns with orthogonal or similar selectivity. These results of column selectivities were compared with those obtained by geometric orthogonality approach, and a consistent result was acquired. Finally, Click TE-CD and XCharge C18PN with highest difference in column selectivity were applied to the separation of Psoralea corylifolia extraction.

Hydrophilic interaction chromatography for selective separation of isomeric saponins

Co-reporter:Xiujie Guo, Xiuli Zhang, Zhimou Guo, Yanfang Liu, Aijin Shen, Gaowa Jin, Xinmiao Liang

Journal of Chromatography A 2014 Volume 1325() pp:121-128

Publication Date(Web):17 January 2014

DOI:10.1016/j.chroma.2013.12.006

•An efficient HILIC method was developed to separate isomeric saponins.•A Click XIon column with improved hydrophilicity and polar selectivity was used.•Methanol was the weak eluent, and symmetrical peak in high sample loading was obtained.•Eleven saponins were isolated and identified.•A new saponin has been isolated and identified.A method based on a Click XIon zwitterionic stationary phase was developed to separate isomeric saponins efficiently in hydrophilic interaction chromatography (HILIC) mode using methanol as a weak eluent. The retention times of a set of isomeric saponins, ginsenoside Rc (S1), ginsenoside Rb2 (S2), and ginsenoside Rb3 (S3) on five kinds of HILIC columns were compared using acetonitrile/water or methanol/water as mobile phase. All results indicated that the Click XIon column showed the highest retention times of all these isomeric saponins. Then the retention behaviors of these isomeric saponins on the Click XIon column were investigated. The results demonstrated that the retention behaviors of saponins on Click XIon in methanol/water mobile phase were different from that in acetonitrile/water. Methanol/water binary eluent offered enhanced selectivity to these isomeric saponins (αS2/S3(MeOH) = 1.16 > αS3/S2(ACN) = 1.04), and the elution order of ginsenoside Rb2 (S2) and ginsenoside Rb3 (S3) was reversed compared with acetonitrile/water. Moreover, methanol/water solvent has better solubility for saponins than acetonitrile/water, resulting in improved preparative peak shape, which is greatly beneficial for saponin purification. Application to the preparative separation of saponins from leaves of P. notoginseng was also investigated, and eleven saponins, including three sets of isomeric saponins with one new saponin were isolated and identified. All these results indicated that this method was efficient for analytical and preparative separation of saponins, especially for isomeric saponins, containing xylopyranosyl, arabinofuranosyl or arabinopyranosyl units.

Hydrophilic interaction liquid chromatography-solid phase extraction directly combined with protein precipitation for the determination of triptorelin in plasma

Co-reporter:Jixia Wang, Song Kong, Jingyu Yan, Gaowa Jin, Zhimou Guo, Aijin Shen, Junyan Xu, Xiuli Zhang, Lijuan Zou, Xinmiao Liang

Journal of Chromatography B 2014 960() pp: 214-221

Publication Date(Web):

DOI:10.1016/j.jchromb.2014.04.036

Selective separation and purification of highly polar basic compounds using a silica-based strong cation exchange stationary phase

Co-reporter:Zhen Long, Zhimou Guo, Xingya Xue, Xiuli Zhang, Lilly Nordahl, Xinmiao Liang

Analytica Chimica Acta 2013 Volume 804() pp:304-312

Publication Date(Web):4 December 2013

DOI:10.1016/j.aca.2013.10.034

•The current method is developed for very polar basic compounds.•The symmetric peak shape of very polar basic compounds can be obtained.•Separation conditions in SCX mode were systematically investigated.Compared to moderately and weakly hydrophilic bases, highly polar basic compounds are even more difficult to separate due to their poor retention in reversed phase (RP) mode. This study described the successful applications of a strong cation exchange (SCX) stationary phase to achieve symmetric peak shape, adequate retention and selectivity in the separation of very polar basic compounds. Salt and acetonitrile concentrations were adjusted to optimize the separation. Good correlations (R2 = 0.998–1.000) between the logarithm of the retention factor and the logarithm of salt or acetonitrile concentration were obtained. Gradients generated by changing salt or acetonitrile concentration were compared for the analysis of different highly polar bases. Although all of the analytes were eluted more quickly with an acetonitrile gradient, the effect of the gradients tested on peak width and peak shape varied with respect to analyte. In addition, the effects of different types of cation and anion additives were also investigated. After separation parameters were acquired, the SCX-based method was utilized to analyze highly hydrophilic alkaloids from Scopolia tangutica Maxim with high separation efficiency (plate numbers > 32,000 m−1). Concurrently, one very polar alkaloid fraction was purified with symmetric peak shape using the current method. Our results suggest that SCX stationary phase can be used as an alternative to RP stationary phase in the analysis and purification of highly hydrophilic basic compounds.

Overloading study of basic compounds with a positively charged C18 column in liquid chromatography

Co-reporter:Chaoran Wang, Zhimou Guo, Zhen Long, Xiuli Zhang, Xinmiao Liang

Journal of Chromatography A 2013 Volume 1281() pp:60-66

Publication Date(Web):15 March 2013

DOI:10.1016/j.chroma.2013.01.074

While tailing and overloading of basic compounds remain problematic on most RP columns, a new kind of positively charged RP column named XCharge C18 was found to be superior good for the separation of alkaloids in our practical use. In this work, the surface charge property of the XCharge C18 column was evaluated by the retention of NO3− under different pH values and buffer concentrations. A considerable and pH-dependent positive charge was confirmed on the column. Then overloading behaviors of bases were systematically studied using amitriptyline as a basic probe. Good peak shapes (Tf < 1.5) and extra high loadability with a C0.5 of about 30,000 mg/L were observed on the column, with commonly used 0.1% formic acid as mobile phase additive. However, increasing the ionic strength of buffer with phosphates led to tailing peaks at high sample amount and sharp decline in loadability (C0.5 of 2000–3000 mg/L), although it brought higher column efficiency at low sample amount. Higher pH also induced worse performance and lower loadability. The overall results demonstrated the importance of an appropriate level of ionic repulsion for the XCharge C18 column to achieve the good performance for bases, which could be explained by the multiple-site adsorption theory as ionic repulsion would shield the solute from occupying high-energy sites deeper in C18 layer.Highlights► Considerable positive charge was proved on XCharge C18. ► Strikingly higher loadability of bases for XCharge C18 was obtained. ► The good loadability was closely related to the charge property.

Orthogonal separation and identification of long-chain peptides from scorpion Buthus martensi Karsch venom by using two-dimensional mixed-mode reversed phase-reversed phase chromatography coupled to tandem mass spectrometry

Co-reporter:Junyan Xu, Xiuli Zhang, Zhimou Guo, Jingyu Yan, Long Yu, Xiuling Li, Xingya Xue and Xinmiao Liang

Analyst 2013 vol. 138(Issue 6) pp:1835-1843

Publication Date(Web):08 Jan 2013

DOI:10.1039/C2AN36704A

Peptide components of scorpion venom have been employed as useful pharmacological tools in the study of ion channel function. The isolation of individual components is necessary for determination of their biological significance. Here, we have described a novel reversed phase (RP)/ion exchange stationary phase, Click oligo ethylene glycol (Click OEG), and the chromatographic efficiency of its mixed-mode sorbent in peptide separation experiments. The Click OEG presents a mixed-mode RP/weak anion-exchange type stationary phase at pH 3.5 and mixed-mode RP/weak cation-exchange type stationary phase at pH 6.0, and it was suitable for separation of long-chain peptides in scorpion venom. Subsequently, a two dimensional mixed-mode RP–RP system based Click OEG and C18 with different pH values in two dimensions was developed for orthogonal separation of scorpion venom. Furthermore, two fractions were analyzed in depth, and 11 long-chain peptides were purified and sequences were identified by using tandem mass spectrometry incorporating the tryptic approach. Among these, we isolated six novel peptides including one peptide with a new sequence and five transcript-level peptides, and speculated on their possible bioactivities.

Two-dimensional strong cation exchange/positively charged reversed-phase liquid chromatography for alkaloid analysis and purification

Co-reporter:Zhen Long;Zhimou Guo;Xingya Xue;Xinmiao Liang

Journal of Separation Science 2013 Volume 36( Issue 24) pp:3845-3852

Publication Date(Web):

DOI:10.1002/jssc.201300863

Peak tailing and nonalkaloid coelution usually hinder alkaloid purification. In this study, a 2DLC, strong cation exchange (SCX) coupled with positively charged RP (PGRP) LC, was developed to overcome these problems. Ten compounds including basic and nonbasic compounds were analyzed. Nonbasic compounds, which are coeluted with basic compounds on RP or PGRP columns, were weakly retained on the SCX column. In addition, a symmetrical peak shape (tailing factors <1.2) of basic compounds can be obtained in the current system. Compared to two other 2D systems, the current system provided the highest orthogonality (R² = 0.045). Furthermore, the SCX coupled with PGRP system was applied for alkaloid purification from a traditional Chinese medicine. Nineteen alkaloids were obtained and one of them was identified as a novel compound. The overall results demonstrate that the proposed system is a powerful tool for alkaloid purification.

Two-dimensional liquid chromatography separation of peptides using reversed-phase/weak cation-exchange mixed-mode column in first dimension

Co-reporter:Xiaoming Cai, Zhimou Guo, Xingya Xue, Junyan Xu, Xiuli Zhang, Xinmiao Liang

Journal of Chromatography A 2012 Volume 1228() pp:242-249

Publication Date(Web):9 March 2012

DOI:10.1016/j.chroma.2011.06.042

Selection of a first-dimensional separation method is very important in proteomic studies performed with two-dimensional liquid chromatography (2D-LC), since reversed-phase chromatography (RPLC) is usually chosen as the second-dimensional separation method in most studies. In this paper, we assess the potential use of mixed-mode reversed-phase/weak cation-exchange (RP/WCX) chromatography in 2D-LC proteomic studies. First, a new RP/WCX mixed-mode stationary phase (named C18WCX) was synthesized based on the polar-copolymerized approach, and a C18WCX column with separation efficiency comparative to conventional C18 columns was developed. This new mixed-mode column primarily provides hydrophobic interactions under acidic condition, but can offer hydrophobic and cation-exchange interactions under neutral and weak basic conditions. An off-line 2D-RP/WCX–RPLC system was established using the C18WCX column with a mobile phase of pH 6.5 in the first dimension and a C18 column with a mobile phase of pH 3.0 in the second dimension. The orthogonality of this two-dimensional system, evaluated through the separation of 123 tryptic peptides, was shown to be higher than that of the conventional 2D-RP–RPLC approach. Applying this 2D-LC method to rat brain samples, we identified 1031 proteins and 4397 unique peptides. In addition, this new two-dimensional method improved the identification of basic peptides. Therefore, we propose that this novel 2D-RP/WCX–RPLC system can be used as an alternative approach for the two-dimensional separation of peptides.

A non-aqueous solid phase extraction method for alkaloid enrichment and its application in the determination of hyoscyamine and scopolamine

Co-reporter:Zhen Long, Chaoran Wang, Zhimou Guo, Xiuli Zhang, Lilly Nordahl, Jing Zeng, Jianguo Zeng and Xinmiao Liang

Analyst 2012 vol. 137(Issue 6) pp:1451-1457

Publication Date(Web):02 Feb 2012

DOI:10.1039/C2AN15824H

A non-aqueous solid phase extraction (SPE) method utilizing silica based strong cation exchange (SCX) was developed and optimized for the enrichment of alkaloids. In this method, silica based SCX SPE columns were used for the elimination of non-alkaloid compounds and the preconcentration of alkaloids from the extracts. Mass spectrometry was employed to analyze the alkaloid-enriched fraction, and results showed that the SPE method developed in this study was effective for the removal of non-alkaloids. Then, this pretreatment method was combined with high performance liquid chromatography for the quantification of scopolamine and hyoscyamine from Scopolia tangutica Maxim. The recoveries of scopolamine and (−)-hyoscyamine were 98.51% and 91.12%, respectively. Relative standard deviation values were 1.4% for scopolamine and 1.6% for (−)-hyoscyamine. The linearity was good in the 0.01–0.8 mg mL−1 range for hyoscyamine and 0.01–0.4 mg mL−1 range for scopolamine.

Application of matrix solid-phase dispersion methodology to the extraction of endogenous peptides from porcine hypothalamus samples for MS and LC–MS analysis

Co-reporter:Xiaoming Cai, Chaoran Wang, Junyan Xu, Xingya Xue, Xiuli Zhang, Xinmiao Liang

Journal of Chromatography B 2011 Volume 879(9–10) pp:657-661

Publication Date(Web):15 March 2011

DOI:10.1016/j.jchromb.2011.01.038

In this study, we investigated a novel application of matrix solid-phase dispersion (MSPD) methodology for the extraction of endogenous peptides from porcine hypothalamus tissue samples. Several experimental factors of the MSPD procedure were examined. Finally, silica-based octadecyl was chosen as dispersing material and blended with 0.25 g porcine hypothalamus at a ratio of 5, and 10 mL of 60% acetonitrile with 0.2% formic acid in water was chosen as the extraction and elution solvent. This MSPD extraction method was compared to the classic acid extraction method. More peaks were observed in the MSPD extracts (74 ± 5) by MALDI-TOF MS than in acid extracts (34 ± 5). Moreover, 14 potential endogenous peptides were identified in the MSPD extracts after nanoLC–MS/MS analysis, while only 2 endogenous peptides in the acid extracts. These results indicated that MSPD could be employed as a simple and efficient method for the extraction of endogenous peptides from tissues.

Metabonomic Study of Lung Cancer and the Effects of Radiotherapy on Lung Cancer Patients: Analysis of Highly Polar Metabolites by Ultraperformance HILIC Coupled with Q-TOF MS

Co-reporter:Xiaoming Cai;Jun Dong;Lijuan Zou;Xingya Xue

Chromatographia 2011 Volume 74( Issue 5-6) pp:

Publication Date(Web):2011 September

DOI:10.1007/s10337-011-2077-4

In this study, plasma samples were collected from 28 health volunteers and 66 lung cancer patients. Ultraperformance HILIC/Q-TOF MS-based metabonomic techniques were employed to compare the highly polar metabolites (HPMs) in the plasma of patients with lung cancer and those in the plasma of healthy volunteers. High separation efficiency and good repeatability of the HILIC/Q-TOF MS method were observed. Partial least squares discriminant analysis (PLS-DA) of the data from both ESI+ and ESI− mode revealed good classifications between the health volunteer and the lung cancer patients. This result showed that the HPMs from lung cancer patients and healthy controls were significantly different. The correct classification rate of models in both ion modes reached 100%, indicating that the metabonomics method established in this study could predict the plasma samples with high accuracy. Besides, we found 19 ions that show a significant difference in levels between lung cancer patients and healthy controls. Finally, we conducted a primary study of the effect of radiotherapy on HPMs in lung cancer patients. Clear differences among the HPMs of patients in different radiotherapy periods and significant changes in levels of the 19 ions after radiotherapy were noted. This demonstrated that radiotherapy influences the metabolism system of patients.

Purification of active bufadienolides from toad skin by preparative reversed-phase liquid chromatography coupled with hydrophilic interaction chromatography

Co-reporter:Yanfang Liu;Jiatao Feng;Yuansheng Xiao;Zhimou Guo;Jing Zhang;Xingya Xue;Jin Ding;Xinmiao Liang

Journal of Separation Science 2010 Volume 33( Issue 10) pp:1487-1494

Publication Date(Web):

DOI:10.1002/jssc.200900848

Abstract

An isolation method by reversed-phase liquid chromatography coupled with hydrophilic interaction chromatography was successfully used to isolate and purify active bufadienolides from Bufo bufo gargarizans Cantor toad skin. In the first step, crude samples were run on an XTerra Prep C18 column. After screening for activity, two fractions were chosen for further purification. A Click β-Cyclodextrin (Click-CD) column made in our laboratory was used for the second step. Seven compounds, including four stereoisomers, were obtained at high purity. The orthogonal isolation method described here was a powerful tool for isolating bufadienolides, including stereoisomers, from a natural product. This integrated method may be useful for the discovery of novel active compounds from natural products.

Purification of polar compounds from Radix isatidis using conventional C18 column coupled with polar-copolymerized C18 column

Co-reporter:Jing Zeng;Zhimou Guo;Yuansheng Xiao;Chaoran Wang, ;Xinmiao Liang

Journal of Separation Science 2010 Volume 33( Issue 21) pp:3341-3346

Publication Date(Web):

DOI:10.1002/jssc.201000417

Abstract

Regarding hydrophilic interaction chromatography and normal phase liquid chromatography, RPLC is another choice used to separate polar compounds with the improvement of polar-modified C18 stationary phase. In this study, a method using conventional C18 column coupled with polar-copolymerized C18 column was successfully developed for the separation and purification of polar compounds from Radix isatidis, which is one of the most commonly used traditional Chinese medicines (TCMs). An XTerra MS C18 column was used to fractionate the extract of R. isatidis and a homemade polar-copolymerized C18 column was utilized for the final purification due to its good separation selectivity and high resolution for polar compounds. The established purification system demonstrated good orthogonality for the polar compounds. As a result, ten compounds were purified and three of them were identified as 3-methyl-5-vinyloxazolidin-2-one (compound A), 5-hydroxymethyl-2-furaldehyde (compound B) and 3-methylfuran-2-carboxylic acid (compound G) based on the MS, IR and extensive NMR data, respectively. It was demonstrated to be a feasible and powerful technique for the purification of polar compounds under RPLC mode and more chemical information of TCMs will be obtained to interpret the efficiency of TCMs.

Lysophosphatidylcholine profiling of plasma: discrimination of isomers and discovery of lung cancer biomarkers

Co-reporter:Jun Dong;Xiaoming Cai;Lili Zhao;Xingya Xue;Lijuan Zou

Metabolomics 2010 Volume 6( Issue 4) pp:478-488

Publication Date(Web):2010 December

DOI:10.1007/s11306-010-0215-x

Lysophosphatidylcholines (lysoPCs) are a class of compounds that have a constant polar head, and fatty acyls of different chain lengths, position, degrees of saturation, and double bond location in human plasma. LysoPCs levels can be a clinical diagnostic indicator that reveals pathophysiological changes. In this work, a method was developed to discriminate between different types of lysoPCs using reversed phase ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry, using mass spectrometry MSE. Isomeric lysoPCs were distinguished based on retention time and the peak intensity ratio of product ions, and 14 pairs of lysoPCs regioisomers were identified in human plasma. The plasma samples of 12 lung cancer patients and 12 healthy persons were collected and analyzed by principal component analysis to generate metabolic profiles of the identified lysoPCs. Both electrospray ionization ESI+ and ESI− results showed that all lung cancer patients had the same five lysoPC metabolic abnormalities, specifically in sn-1 lyso16:0, sn-2 lysoPC 16:0, sn-1 lysoPC 18:0, sn-1 lysoPC 18:1 and sn-1 lysoPC 18:2. Thus, the function of isomers with different fatty acyl positions may be related to lung cancer, and this may help elucidate the mechanism of the disease.

Selectively preparative purification of aristolochic acids and aristololactams from Aristolochia plants

Co-reporter:Jing Zhang, Yuansheng Xiao, Jiatao Feng, Sophia L. Wu, Xingya Xue, Xiuli Zhang, Xinmiao Liang

Journal of Pharmaceutical and Biomedical Analysis 2010 52(4) pp: 446-451

Publication Date(Web):

DOI:10.1016/j.jpba.2010.01.023

Analysis of highly polar metabolites in human plasma by ultra-performance hydrophilic interaction liquid chromatography coupled with quadrupole-time of flight mass spectrometry

Co-reporter:Xiaoming Cai, Lijuan Zou, Jun Dong, Lili Zhao, Yuanyuan Wang, Qing Xu, Xingya Xue, Xiuli Zhang, Xinmiao Liang

Analytica Chimica Acta 2009 Volume 650(Issue 1) pp:10-15

Publication Date(Web):14 September 2009

DOI:10.1016/j.aca.2009.01.054

Highly polar metabolites are abundant in human plasma. Analysis of these compounds by standard reverse-phase chromatography is difficult. Highly polar metabolites were extracted by a two-step method. They were analyzed by ultra-performance hydrophilic interaction chromatography (HILIC) coupled to quadrupole-time of flight mass spectrometer detection technology. The middle and low polar fraction were also analyzed using a standard C18 column. Data were extracted by Markerlynx, and analyzed by multivariate statistical methods to discriminate human plasma samples by sex and age. The results not only showed good classification of samples by sex and age, but also revealed new potential biomarkers not revealed by standard RPLC/MS analysis. This study showed that HILIC is an effective technique to analyze highly polar metabolites for metabonomic studies.

Purification of alkaloids from Corydalis yanhusuo W. T. Wang using preparative 2-D HPLC

Co-reporter:Jing Zhang;Yu Jin;Yanfang Liu;Yuansheng Xiao;Jiatao Feng;Xingya Xue ;Xinmiao Liang

Journal of Separation Science 2009 Volume 32( Issue 9) pp:1401-1406

Publication Date(Web):

DOI:10.1002/jssc.200800729

Abstract

Two-dimensional preparative multi-channel parallel high performance liquid chromatography was successfully applied for the first time to isolate and purify alkaloids from Corydalis yanhusuo. The experiments were performed in off-line mode using the same preparative chromatographic column with pH 3.5 in the first and pH 10.0 in the second separation dimension. In the preparative process, UV-triggered fraction collection was used in the first dimension while UV and MS-triggered collection were used in the second dimension for reasons of sensitivity and complementarity. Two pure compounds and nine fractions were obtained in the first dimension. Then two representative fractions were further purified in the second dimension and six pure compounds were obtained. The results demonstrated that this procedure is an effective approach for the preparative isolation and purification of alkaloids from Corydalis yanhusuo. Based on the different pH values of the mobile phase in this method, it is also suitable for the preparative isolation and purification of other compounds from TCMs which are sensitive to the pH of the solutions. Moreover, this method will be a promising tool for the purification of low content compounds from natural products.

Systematic screening and characterization of tertiary and quaternary alkaloids from corydalis yanhusuo W.T. Wang using ultra-performance liquid chromatography–quadrupole-time-of-flight mass spectrometry

Co-reporter:Jing Zhang, Yu Jin, Jun Dong, Yuansheng Xiao, Jiatao Feng, Xingya Xue, Xiuli Zhang, Xinmiao Liang

Talanta 2009 Volume 78(Issue 2) pp:513-522

Publication Date(Web):30 April 2009

DOI:10.1016/j.talanta.2008.12.002

Ultra-performance liquid chromatography–quadrupole-time-of-flight mass spectrometry (UPLC–Q-TOF-MS) is an effective technique for analysis of complex samples with offering rapid, efficient separation in combination with accurate mass measurement and tandem mass spectrometry (MS/MS). This paper exploits this technique to identify the alkaloids in corydalis yanhusuo, an important antalgic Traditional Chinese Medicine (TCM). The mass spectral fragmentation behavior of one tertiary alkaloid and two quaternary alkaloids was studied in detail. Low-abundance product ions of tertiary and quaternary alkaloids were investigated and compared between each other. Sixteen alkaloids were screened out by using a systematic screening method developed in our laboratory; structures of eight therein were identified by characteristic UV absorption spectrum and positive ion mode of Q-TOF-MS/MS; and two of them were discovered for the first time in corydalis yanhusuo to our knowledge. This research demonstrates the potential of UPLC-Q-TOF-MS in structural characterization and identification of components in traditional Chinese herbal medicines.

UPLC/Q-TOFMS/MS as a powerful technique for rapid identification of polymethoxylated flavones in Fructus aurantii

Co-reporter:Da-Yong Zhou, Xiu-Li Zhang, Qing Xu, Xing-Ya Xue, Fei-Fang Zhang, Xin-Miao Liang

Journal of Pharmaceutical and Biomedical Analysis 2009 50(1) pp: 2-8

Publication Date(Web):

DOI:10.1016/j.jpba.2009.03.010

Characterization of anthocyanins in wild Lycium ruthenicum Murray by HPLC-DAD/QTOF-MS/MS

Co-reporter:

Analytical Methods (2009-Present) 2015 - vol. 7(Issue 12) pp:NaN4956-4956

Publication Date(Web):2015/05/06

DOI:10.1039/C5AY00612K