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COMPREHENSIVE TWO-DIMENSIONAL LIQUID CHROMATOGRAPHY COUPLED WITH QUADRUPLE TIME-OF-FLIGHT MASS SPECTROMETRY FOR CHEMICAL CONSTITUENTS ANALYSIS OF TRIPTERYGIUM GLYCOSIDES TABLETS 被引量:11
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作者 Xiao Yao 《World Journal of Traditional Chinese Medicine》 2015年第4期66-66,共1页
Comprehensive two-dimensional liquid chromatography platform(LC×LC)coupled with quadrupole time-of-flight(QTOF)mass spectrometry(MS)is developed to separate,identify and relatively determine the chemical constitu... Comprehensive two-dimensional liquid chromatography platform(LC×LC)coupled with quadrupole time-of-flight(QTOF)mass spectrometry(MS)is developed to separate,identify and relatively determine the chemical constituents of two types of tripterygium glycosides tablets(TGT).The types and relative contents of the constituents discovered in two kinds of TGT tablets were subsequently compared.C8andC18 column were used for the separation of the first 展开更多
关键词 TGT comprehensive two-dimensional liquid chromatography COUPLED WITH QUADRUPLE TIME-OF-FLIGHT MASS SPECTROMETRY FOR CHEMICAL CONSTITUENTS ANALYSIS OF TRIPTERYGIUM GLYCOSIDES TABLETS
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Offline two-dimensional liquid chromatography coupled with ion mobility-quadrupole time-of-flight mass spectrometry enabling fourdimensional separation and characterization of the multicomponents from white ginseng and red ginseng 被引量:10
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作者 Tiantian Zuo Chunxia Zhang +7 位作者 Weiwei Li Hongda Wang Ying Hu Wenzhi Yang Li Jia Xiaoyan Wang Xiumei Gao Dean Guo 《Journal of Pharmaceutical Analysis》 SCIE CAS CSCD 2020年第6期597-609,共13页
Inherent complexity of plant metabolites necessitates the use of multi-dimensional information to accomplish comprehensive profiling and confirmative identification.A dimension-enhanced strategy,by offline two-dimensi... Inherent complexity of plant metabolites necessitates the use of multi-dimensional information to accomplish comprehensive profiling and confirmative identification.A dimension-enhanced strategy,by offline two-dimensional liquid chromatography/ion mobility-quadrupole time-of-flight mass spectrometry(2 D-LC/IM-QTOF-MS)enabling four-dimensional separations(2 D-LC,IM,and MS),is proposed.In combination with in-house database-driven automated peak annotation,this strategy was utilized to characterize ginsenosides simultaneously from white ginseng(WG)and red ginseng(RG).An offline 2 DLC system configuring an Xbridge Amide column and an HSS T3 column showed orthogonality 0.76 in the resolution of ginsenosides.Ginsenoside analysis was performed by data-independent high-definition MSE(HDMSE)in the negative ESI mode on a Vion?IMS-QTOF hybrid high-resolution mass spectrometer,which could better resolve ginsenosides than MSEand directly give the CCS information.An in-house ginsenoside database recording 504 known ginsenosides and 58 reference compounds,was established to assist the identification of ginsenosides.Streamlined workflows,by applying UNIFI?to automatedly annotate the HDMSEdata,were proposed.We could separate and characterize 323 ginsenosides(including 286 from WG and 306 from RG),and 125 thereof may have not been isolated from the Panax genus.The established 2 D-LC/IM-QTOF-HDMSEapproach could also act as a magnifier to probe differentiated components between WG and RG.Compared with conventional approaches,this dimensionenhanced strategy could better resolve coeluting herbal components and more efficiently,more reliably identify the multicomponents,which,we believe,offers more possibilities for the systematic exposure and confirmative identification of plant metabolites. 展开更多
关键词 Dimension-enhanced strategy Multicomponent characterization GINSENOSIDE Offline two-dimensional liquid chromatography Ion mobility-quadrupole time-of-flight mass spectrometry In-house database
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Establishing a protein expression profile database for the normal human pituitary gland using two-dimensional high-performance liquid chromatography combined with LTQ-Orbitrap mass spectrometry 被引量:2
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作者 Rong Xie Wei Xu +4 位作者 Weimin Bao Hang Liu Luping Chen Yiwen Shen Jianhong Zhu 《Neural Regeneration Research》 SCIE CAS CSCD 2012年第36期2922-2928,共7页
In this study, we selected adult normal pituitary gland tissues from six patients during operations for pituitary microadenomas via the transsphenoidal approach for extended normal pituitary tissue resection around th... In this study, we selected adult normal pituitary gland tissues from six patients during operations for pituitary microadenomas via the transsphenoidal approach for extended normal pituitary tissue resection around the tumor, and analyzed the protein expression of human normal pituitary using two-dimensional high-performance liquid chromatography combined with LTQ-Orbitrap mass spectrometry proteomics technology. The ten most highly expressed proteins in normal human pituitary were: alpha 3 type VI collagen isoform 5 precursor (abundance among tall pituitary proteins 1.30%), fibrinogen beta chain preproprotein (0.99%), vimentin (0.73%), prolactin (0.69%), ATP synthase, H~ transporting and mitochondrial F1 complex beta subunit precursor (0.52%), keratin I (0.49%), growth hormone (0.45%), carbonic anhydrase I (0.40%), heat shock protein 90 kDa I (0.31%), and annexin V (0.30%). Based on the biological function classifications of these proteins, the top three categories by content were neuroendocrine proteins (abundance among all pituitary proteins, 40.1%), catalytic and metabolic proteins (28.3%), and cell signal transduction proteins (9.8%). Based on cell positioning classification, the top three categories were cell organelle (24.5%) membrane (20.8%), and cytoplasm (13.0%). Based on biological process classification, the top three categories of proteins are involved in physiological processes (42.9%), cellular processes (40.4%), and regulation of biological processes (9.1%). Our experimental findings indicate that a protein expression profile database of normal human pituitary can be precisely and efficiently established by proteomics technology. 展开更多
关键词 two-dimensional high-performance liquid chromatography mass spectrum pituitary gland PROTEINS PROTEOMICS hypophyseal tumor physiological function pathological mechanism
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Identification of petroleum aromatic fraction by comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry 被引量:6
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作者 WANG HuiTong WENG Na +3 位作者 ZHANG ShuiChang ZHU GuangYou CHEN JianPing WEI CaiYun 《Chinese Science Bulletin》 SCIE EI CAS 2010年第19期2039-2045,共7页
Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry(GC×GC-TOFMS) is commercially available in the 1990s,with the characteristics of large peak capacity,high resolution,h... Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry(GC×GC-TOFMS) is commercially available in the 1990s,with the characteristics of large peak capacity,high resolution,high sensitivity,etc.However,its application to the petroleum and geological analyses is just emerging in China and overseas.In this research,the analytical method for petroleum aromatic fraction using GC×GC-TOFMS is set up,via the choice of the column system and optimization of setting parameters,such as temperature programming,modulation time,hot pulse time,flow rate of carrier gas,data acquisition rate and data processing.The results indicate that different polar compounds of aromatic fraction distribute as bands on structured GC×GC chromatogram.Within each band,homologous compounds appear as a roof-tile structure based on the number of substituent residues.The aromatic compounds are identified and characterized according to the GC×GC chromatogram and mass spectra.According to the polarity and the number of rings,aromatic compounds are spatially present on one chromatogram,which directly reflects the distribution characteristics of complex compounds of aromatic hydrocarbons.In addition,quantitative analysis is favored as some overlapped peaks on traditional GC-MS chromatogram have been separated completely on GC×GC.Some heterocyclic atom aromatic compounds at trace level can be clearly identified using this method,for polarity differences from other interfered aromatic compounds.The development of this method and chromatogram recognition offer petroleum geologists a practical example for the application performance of GC×GC-TOFMS. 展开更多
关键词 comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry aromatic compounds heterocycliccompounds petroleum geological experiments
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Comparison of geochemical parameters derived from comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry and conventional gas chromatography-mass spectrometry 被引量:5
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作者 WANG HuiTong WENG Na +2 位作者 ZHANG ShuiChang ZHU GuangYou WEI CaiYun 《Science China Earth Sciences》 SCIE EI CAS 2011年第12期1892-1901,共10页
The saturated and aromatic hydrocarbon fractions of crude oil samples have been analyzed by using comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (GCxGC-TOFMS) and conventional... The saturated and aromatic hydrocarbon fractions of crude oil samples have been analyzed by using comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (GCxGC-TOFMS) and conventional gas chro- matography-mass spectrometry (GC-MS). In order to investigate the consistency and discrepancy of the obtained data from the two instruments, some petroleum geochemical parameters have been compared. A comparison of 23 geochemical parameters indicates that 10 parameters are comparable from the two instruments with less than 5% deviations. Therefore, GCxGC-TOFMS is equivalent to conventional GC-MS in some geochemical parameter acquisitions. However, the other 13 parameters are discrepant, including gammacerane / αβ-hopane, Ts/Tm, 2-ethyl-naphthalene / 1-ethyl-naphthalene (ENR), (2, 6-dimethyl-naphthalene +2,7-dimethyl-naphthalene) / 1,5-dimethyl-naphthalene (DNR), etc. Furthermore, compared to GCxGC-TOFMS, some low concentration compounds could not be detected by the conventional GC-MS, which results in the missing of related geochemical data. Normally, this is caused by the limited separation power and peak capacity of the conventional GC column. Besides, the co-eluting peak integrations are also affected significantly due to the incomplete separation of the compounds. Some low concentration compounds might not be detected because of the interference from the baseline noise or from other substances. GCxGC-TOFMS prevails in compound separation against the conventional GC-MS by avoiding co-elution, which achieves more accurate and precise peak area measurement with the presence of a true baseline. So petroleum geochemical parameters obtained from the GCxGC-TOFMS GCxGC-TOFMS may become one of the most effective analytical are more reliable than those from the conventional GC-MS tools for the oil and gas geochemical study. 展开更多
关键词 comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry gas chromatography-mass spectrometry geochemical parameters
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Qualitative Analysis of A Sulfur-fumigated Chinese Herbal Medicine by Comprehensive Two-Dimensional Gas Chromatography and High-Resolution Time of Flight MassSpectrometry Using Colorized Fuzzy Difference Data Processing 被引量:4
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作者 CAI Hao CAO Gang ZHANG Hong-yan 《Chinese Journal of Integrative Medicine》 SCIE CAS CSCD 2017年第4期261-269,共9页
To investigate the chemical transformation of volatile compounds in sulfur-fumigated Radix Angelicae Sinensis. A comprehensive two-dimensional gas chromatography (GCxGC) and high-resolution time-of-flight mass spectro... To investigate the chemical transformation of volatile compounds in sulfur-fumigated Radix Angelicae Sinensis. A comprehensive two-dimensional gas chromatography (GCxGC) and high-resolution time-of-flight mass spectrometry (HR-TOF/MS) with colorized fuzzy difference (CFD) method was used to investigate the effect of sulfur-fumigation on the volatile components from Radix Angelicae Sinensis. Twenty-five compounds that were found in sun-dried samples disappeared in sulfur-fumigated samples. Seventeen volatile components including two sulfur-containing compounds were newly generated for the first time in volatile oils of sulfur-fumigated Radix Angelicae Sinensis. The strategy can be successfully applied to rapidly and holistically discriminate sun-dried and sulfur-fumigated Radix Angelicae Sinensis. GCxGC-HR-TOF/MS based CFD is a powerful and feasible approach for the global quality evaluation of Radix Angelicae Sinensis as well as other herbal medicines. 展开更多
关键词 Radix Angelicae Sinensis comprehensive two-dimensional gas chromatography and high-resolution time-of-flight mass spectrometry colorized fuzzy difference volatile components
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基于肠道菌群和广泛靶向代谢组学的山柰酚抗骨质疏松的作用机制
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作者 梁周 张驰 +7 位作者 潘成镇 杨博 蒲张林 刘桦 彭金辉 文立春 凌观汉 陈锋 《中国组织工程研究》 CAS 北大核心 2025年第20期4190-4204,共15页
背景:山柰酚具有抗骨质疏松的作用,但山柰酚通过调控肠道菌群、代谢物防治骨质疏松的作用机制尚不明确。目的:基于肠道菌群和广泛靶向代谢组学探究山柰酚抗骨质疏松的可能作用机制。方法:将雌性Sprague-Dawley大鼠18只随机分为假手术组... 背景:山柰酚具有抗骨质疏松的作用,但山柰酚通过调控肠道菌群、代谢物防治骨质疏松的作用机制尚不明确。目的:基于肠道菌群和广泛靶向代谢组学探究山柰酚抗骨质疏松的可能作用机制。方法:将雌性Sprague-Dawley大鼠18只随机分为假手术组、模型组和山柰酚组,每组6只,后2组切除双侧卵巢制备骨质疏松大鼠模型。造模后8周,假手术组和模型组采用蒸馏水灌胃,山柰酚组采用40 mg/kg山柰酚灌胃,各组均连续给药12周。取大鼠粪便进行16SrDNA扩增子测序,观察肠道菌群结构的变化;采用超高效液相色谱-串联质谱技术、自主开发的数据库和多元统计分析的方法进行血清样本广泛靶向代谢组学检测。结果与结论:①连续干预12周后,16SrDNA扩增子测序结果显示,与假手术组相比,模型组肠道菌群丰度增加;与模型组相比,山柰酚组上调Latilactobacillus菌属(P=0.021)丰度,下调泛菌属(Pantoea)(P=0.034)、肠杆菌属(Enterorhabdus)(P=0.000)、Monoglobus菌属(P=0.024)、丁酸单胞菌属(Butyricimonas)(P=0.034)、Rothi属(P=0.043)、梭杆菌属(Clostridia)(P=0.004)等菌属丰度。②连续干预12周后,血清样本广泛靶向代谢组学检测结果显示,假手术组与模型组、模型组与山柰酚组之间分别鉴定出120和79种代谢物,3组间共有17种交集差异代谢物,包括乌头酸、巴比妥酸、L-高瓜氨酸、3,4,5-三甲氧基肉桂酸、L-3-苯基乳酸、环(脯氨酸-脯氨酸)、L-苯丙氨酸-L-丝氨酸、脯氨酸-异亮氨酸、L-冬胺基乙酸-L-苯丙胺基乙酸、苯丙氨酸-天冬氨酸等。大部分属于氨基酸及其代谢物、甘油磷脂类和脂肪酰类。差异代谢物涉及的KEGG通路主要富集在D-氨基酸代谢、组氨酸代谢、丙酸代谢、赖氨酸降解、脂肪酸代谢、鞘脂代谢等。③连续干预12周后,联合分析发现,肠杆菌属(Enterorhabdus)、Latilactobacillus属、Rothia属和瘤胃球菌属(Ruminococcus)等与血清差异代谢物密切相关。④山柰酚可能通过调节肠道菌群的丰度、多样性及结构,调控氨基酸及其代谢物的代谢、脂肪酸代谢等发挥抗骨质疏松的作用。 展开更多
关键词 山柰酚 骨质疏松 肠道菌群 16SrDNA扩增子测序 广泛靶向代谢组学 超高效液相色谱-串联质谱 作用机制 大鼠
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Using cell membrane chromatography and HPLC-TOF/MS method for in vivo study of active components from roots of Aconitum carmichaeli 被引量:4
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作者 Yan Cao Xiao- Fei Chen +3 位作者 Di- Ya Lu Xin Dong Guo-Qing Zhang Yi- Feng Chai 《Journal of Pharmaceutical Analysis》 SCIE CAS 2011年第2期125-134,共10页
An offline two-dimensional system combining a rat cardiac mascle cell membrane chromatography time-of-flight mass spectrometry (CMC-TOF/MS) with a high performance liquid chromatography time-of-flight mass spectrome... An offline two-dimensional system combining a rat cardiac mascle cell membrane chromatography time-of-flight mass spectrometry (CMC-TOF/MS) with a high performance liquid chromatography time-of-flight mass spectrometry (HPLC-TOF/MS) was established for investigating the parent components and metabolites in rat urine samples after administration of the roots of Aconitum carmichaeli. On the basis of the analysis of the first dimension, retention components of the urine sample were collected into 30 fractions (one fraction per minute). Then offline analysis of the second dimension was carried out. 34 compounds including 24 parent alkaloids and 10 potential metabolites were identified from the dosed rat urine, and then binding affinities of different compounds on cell membranes were compared and influences of some functional groups on activity were estimated with the semi-quantification and curve fitting method. As a result, binding affinities decreased along with the process of deacylation, debenzoylation and demethylation, which may be related to the alleviation of toxicity in the procedure of herb processing or metabolism. Moreover, some minor components in rat urine (Songorine, 14-benzoylneoline, Deoxyaconitine, etc. ) exerted relatively strong affinity on cell membranes are worth exploring. The results delivered by the system suggest that the CMC can be applied to in vivo study. 展开更多
关键词 cell membrane chromatography high performance liquid chromatography time-of-flight mass spectrometry two-dimensional system Aconitum carmichaeli
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On-line parallel reversed phase two-dimensional liquid chromatography for high-throughput analysis of complex proteomic samples 被引量:2
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作者 WANG Zhicong1,3, ZHANG Qinghe2, LI Tong2, ZHAO Zhongyi3 & ZHANG Weibing1 1. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116011, China 2. Dalian Elite Analytical Instrument Co., Ltd., Dalian 116011, China 3. Faculty of Material Science and Chemical Engineering, China University of Geosciences, Wuhan 430074, China 《Science China Chemistry》 SCIE EI CAS 2006年第6期527-533,共7页
A comprehensive two-dimensional liquid chromatographic system (2D SCX/RP) is con- structed with a 10-port-2-way valve using strong cation exchange chromatography (Hypersil SCX, 100 mm×4.6 mm I.D.) followed by rev... A comprehensive two-dimensional liquid chromatographic system (2D SCX/RP) is con- structed with a 10-port-2-way valve using strong cation exchange chromatography (Hypersil SCX, 100 mm×4.6 mm I.D.) followed by reversed phase chromatography (Hypersil BDS C18, 15 mm×4.6 mm I.D.) to separate the complex peptides from globin peptic hydrolysate. After the sample was loaded on the SCX column, the phosphate buffer (pH 4.0) was used to elute the peptides. Then, elutes flowed through the interface and the peptides focused on the head of the trapping columns (Hypersil BDS C18, 15 mm×4.6 mm I.D.) but salt passed into the waste. After the valve was switched, the samples were flushed with a backward flow into the RP analytical column. The peptides on the SCX were eluted with 12 discontinuous steps linearly increasing salt concentrations. The peptides enriched on the trapping column were desalted and separated by the RP columns. The resolution and the resolved peaks of the 2D SCX/RP system were greatly increased and the total peak capacity reached as high as 2280. 展开更多
关键词 two-dimensional liquid chromatography interface TRAPPING column proteomics globin.
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Double Off-line Two-dimensional Liquid Chromatography for Separation and Identification of Compounds in Salvia Miltiorrhiza(Danshen) 被引量:3
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作者 Ji-xia Wang Xiu-li Zhang +5 位作者 Fan Yang Hong-li Jin Li-ying Shi Wei-jia Zhou Yan-fang Liu Xin-miao Liang 《World Journal of Traditional Chinese Medicine》 2015年第3期27-39,共13页
Background: Danshen is an important traditional Chinese medicine(TCM) used for the treatment of cardiovascular and cerebrovascular diseases. Separation and analysis of its components have been widely investigated. How... Background: Danshen is an important traditional Chinese medicine(TCM) used for the treatment of cardiovascular and cerebrovascular diseases. Separation and analysis of its components have been widely investigated. However, the systematical two dimensional liquid chromatography(2D-LC) methods have not been developed to comprehensively separate and characterize its components.Objective: In this work, double off-line 2D-LC methods were aimed to develop for the systematical separation of compounds from Danshen.Methods: Using solid phase extraction(SPE), the Danshen extract was divided into a medium-polar fraction(Sample I) and a weak-polar fraction(Sample Ⅱ) according to their polarities. Based on reversed-phase liquid chromatography(RPLC) and hydrophilic interaction liquid chromatography(HILIC) modes, a 2D-HILIC × RPLC system and a 2D-RPLC × RPLC system were designed for the separation of Sample Ⅰ and Sample Ⅱ, respectively. According to reversed-phase and HILIC columns selectivities characterized in our previous reports, ZIC-HILIC and XTerra C18 were employed to build the 2D-HILIC × RPLC system and Click TE-CD and XTerra C18 for the 2D-RPLC × RPLC system,respectively.Results: The 2D-HILIC × RPLC and 2D-RPLC × RPLC systems exhibited excellent orthogonality for the separation of Sample Ⅰ and Sample Ⅱ,respectively. Their orthogonalities were 88.42% and 63.24%. Based on these double 2D-LC systems combined with mass spectrometry, at least 200 compounds were found and 33 compounds of them were identified, including 16 phenolic acids and 17 diterpenoid quinines.Conclusion: These results suggest that these two off-line 2D-LC methods are effective for the separation and characterization of components in Danshen. 展开更多
关键词 two-dimensional liquid chromatography SEPARATION IDENTIFICATION DANSHEN
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Ion-pair Reversed-phase×Low-pH Reversed-phase Two-dimensional Liquid Chromatography for In-depth Proteomic Profiling
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作者 NIU Wenxue LIU Zheyi +5 位作者 LIU Jing LAI Can ZHANG Tingting ZHAO Heng WANG Guosheng WANG Fangjun 《Chemical Research in Chinese Universities》 SCIE CAS CSCD 2023年第2期260-265,共6页
High-resolution liquid chromatography separation is essential to in-depth proteomic profiling of complex biological samples.Herein,we established an ion-pair reversed-phase×reversed-phase two-dimensional liquid c... High-resolution liquid chromatography separation is essential to in-depth proteomic profiling of complex biological samples.Herein,we established an ion-pair reversed-phase×reversed-phase two-dimensional liquid chromatography(IPRP×RP 2DLC)strategy for comprehensive proteomic analysis.Both RPLC separation dimensions were performed at low pH,with trifluoroacetic acid(TFA)and formic acid(FA)as mobile phase addictive,respectively.As the good separation resolution offered by ion-pairing effect of TFA,the fractionation efficiency was greatly improved with 74.0%peptides identified in just one fraction.Comparing with conventional high pH RP fractionation,the overall separation rate of IPRP was about 1.6 times that of high-pH RP,which increased the number of identified peptides by 21%.Further,2169 proteins and 8540 peptides were confidently identified from crude serum sample by our IPRP×RP 2DLC strategy,exhibiting great potential in clinical proteomics in the future. 展开更多
关键词 two-dimensional liquid chromatography(2DLC) Ion-pair reversed-phase liquid chromatography(IPRP-LC) IPRP×low-pH RP 2DLC PROTEOMICS Mass spectrometry
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TWO-DIMENSIONAL LIQUID CHROMATOGRAPHY(2D-LC) IN THE ANALYSIS OF PHARMACEUTICALS AND AUTHENTICATION OF CHINESE HERBAL MEDICINE
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作者 Sonja Krieger Waldbronn 《World Journal of Traditional Chinese Medicine》 2015年第4期65-65,共1页
One-dimensional liquid chromatography(1D-LC)is routinely applied to the analysis of all kinds of samples in different fields.With the introduction of UHPLC instruments and sub-2micron particle columns,the separation e... One-dimensional liquid chromatography(1D-LC)is routinely applied to the analysis of all kinds of samples in different fields.With the introduction of UHPLC instruments and sub-2micron particle columns,the separation efficiency was greatly improved.To resolve all components of complex samples,however,1D-LC does not provide enough resolving power,or peak capacity.In addition,to separate compounds co-eluting in 1D-LC,increasing the separation efficiency by increasing 展开更多
关键词 LC IN THE ANALYSIS OF PHARMACEUTICALS AND AUTHENTICATION OF CHINESE HERBAL MEDICINE two-dimensional liquid chromatography
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石香薷水提物HPLC特征图谱的研究 被引量:1
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作者 谢娟 王玉玉 +2 位作者 杨子辉 刘秀斌 曾建国 《饲料工业》 CAS 北大核心 2024年第2期109-118,共10页
石香薷药材用于精油提取后的水提液中仍含有大量生物活性物质,具有开发为饲料添加剂的价值,从而实现石香薷资源的综合利用。采用HPLC法,按照优化后的色谱条件对24批石香薷水提取物样品的化学成分进行测定分析。建立了不同产地石香薷水... 石香薷药材用于精油提取后的水提液中仍含有大量生物活性物质,具有开发为饲料添加剂的价值,从而实现石香薷资源的综合利用。采用HPLC法,按照优化后的色谱条件对24批石香薷水提取物样品的化学成分进行测定分析。建立了不同产地石香薷水提物的HPLC特征图谱,共确定8个特征峰,经对照品比对确定特征峰5、7、8分别为野黄芩苷、迷迭香酸和黄芩素-7-甲醚,设定迷迭香酸为参照峰(S峰),特征峰1~8的相对保留时间的规定值分别为0.176、0.444、0.495、0.676、0.765、0.954、1.000、1.618,精密度、重复性和稳定性考察中各特征峰相对保留时间的相对标准偏差(RSD)分别为0.03%~0.57%、0.01%~0.31%、0.04%~0.15%,相对峰面积的RSD分别为0.88%~2.60%、1.39%~3.33%、1.95%~4.54%。该研究建立的HPLC特征图谱具有良好的精密度、稳定性和重复性,为石香薷水提物作为饲料添加剂开发的质量控制提供了依据。 展开更多
关键词 石香薷水提物 高效液相色谱法 特征图谱 资源综合利用 植物提取物饲料添加剂
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二维液相色谱分离鉴定桑葚中多酚类化合物
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作者 贺增洋 佘世科 +4 位作者 徐志强 彭晓萌 孙丽莉 吴攀 许春平 《食品安全质量检测学报》 CAS 2024年第16期292-299,共8页
目的建立一套亲水作用色谱×反相色谱二维液相色谱系统对桑葚中多酚类化合物进行鉴定。方法首先采用单因素实验对色谱系统中一维色谱的流动相A的组成、二维色谱的色谱运行条件以及两维系统接口处的样品环的体积进行优化,然后利用优... 目的建立一套亲水作用色谱×反相色谱二维液相色谱系统对桑葚中多酚类化合物进行鉴定。方法首先采用单因素实验对色谱系统中一维色谱的流动相A的组成、二维色谱的色谱运行条件以及两维系统接口处的样品环的体积进行优化,然后利用优化系统对桑葚中多酚类化合物进行分离鉴定。结果当一维色谱流动相A中乙酸浓度为2.0%、二维色谱流动相流速为3.3 mL/min、二维色谱分析时间为1.3 min、接口处的样品环体积为150μL时,桑葚提取物中多酚类化合物分离效果最好;使用优化后的系统对桑葚提取物中多酚类化合物进行分离鉴定,成功分离鉴定了桑葚提取物中5种酚类化合物。结论本研究的优化方法可行,优化后的系统可以高效、准确分离桑葚提取物中多酚类化合物,为分离鉴定桑葚中多酚类化合物提供了一定的实践基础。 展开更多
关键词 桑葚 多酚类化合物 全二维液相色谱法 亲水作用色谱-反相色谱法
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本科生综合实验:磁性固相萃取-高效液相色谱测定茶叶样品中的苯脲类除草剂
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作者 刘壮 苏瑛 +2 位作者 杨东伟 李丽梅 许旭 《色谱》 CAS CSCD 北大核心 2024年第11期1094-1100,共7页
在教育部推进新农科建设和学科交叉融合的背景下,本研究设计了一项综合化学实验,旨在提升学生在生物质功能材料制备及农药残留检测中的实践技能。实验采用天然丝瓜络合成氮掺杂磁性多孔碳材料,应用于磁性固相萃取(MSPE)技术,结合高效液... 在教育部推进新农科建设和学科交叉融合的背景下,本研究设计了一项综合化学实验,旨在提升学生在生物质功能材料制备及农药残留检测中的实践技能。实验采用天然丝瓜络合成氮掺杂磁性多孔碳材料,应用于磁性固相萃取(MSPE)技术,结合高效液相色谱法(HPLC)检测茶叶样品中的苯脲类除草剂灭草隆。该实验流程包括材料合成、表征、MSPE条件优化、吸附性能研究及HPLC分析,体现了科学性和系统性,为学生提供了一个全面的学习平台。本实验不仅加深了学生对材料特性与应用之间关系的理解,而且提高了实验设计和问题解决能力。通过科学前沿、课程思政与实验教学的结合,不仅激发了学生的科研兴趣,培养了创新思维和实践能力,还加强了学生的社会责任感和历史使命感,实现了实验教学的全面育人目标,为培养具有全球视野和社会责任感的高素质人才奠定了基础。 展开更多
关键词 综合化学实验 磁性固相萃取 高效液相色谱 农药分析 生物质材料
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基于高效液相色谱法多指标定量联合化学计量学及灰色关联度分析评价泻青丸综合质量
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作者 金晓姣 徐磊 +1 位作者 王玉莹 李志国 《中国药物与临床》 CAS 2024年第9期605-612,F0003,共9页
目的建立泻青丸多指标成分定量方法,同时借助化学计量学及灰色关联度分析(GRA)评价其综合质量。方法采用高效液相色谱法(HPLC),以Venusil MP C18为色谱柱,乙腈-0.2%冰醋酸为流动相,同时测定泻青丸中獐牙菜苦苷、龙胆苦苷、獐牙菜苷、山... 目的建立泻青丸多指标成分定量方法,同时借助化学计量学及灰色关联度分析(GRA)评价其综合质量。方法采用高效液相色谱法(HPLC),以Venusil MP C18为色谱柱,乙腈-0.2%冰醋酸为流动相,同时测定泻青丸中獐牙菜苦苷、龙胆苦苷、獐牙菜苷、山栀子苷、羟异栀子苷、京尼平龙胆双糖苷、栀子苷、升麻素苷、升麻素、亥茅酚苷、洋川芎内酯H、洋川芎内酯I、洋川芎内酯A和藁本内酯含量。结合化学计量学挖掘影响泻青丸产品质量的差异标志物。以相对关联度为测度,对泻青丸综合质量进行评价。结果完成14个成分含量测定方法学验证,结果均符合中国药典要求。化学计量学分析显示栀子苷、龙胆苦苷、藁本内酯、京尼平龙胆双糖苷、洋川芎内酯A、升麻素苷和羟异栀子苷是影响泻青丸产品质量的主要因子。GRA结果显示相对关联度为0.385~0.584,可用于泻青丸质量优劣评价。结论HPLC多组分定量与化学计量学及GRA方法结合可综合评价泻青丸质量。 展开更多
关键词 泻青丸 色谱法 液相 化学计量 综合评价
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全二维液相色谱的初步构建及其在山羊血清分离中的应用 被引量:9
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作者 王智聪 张庆合 +2 位作者 张维冰 李彤 赵中一 《分析化学》 SCIE EI CAS CSCD 北大核心 2005年第4期437-441,共5页
以GFC/RP模式构建全二维液相色谱系统,第一维凝胶过滤色谱柱使用ShodexProteinKW 802. 5(300mm×8mmi.d. ),以0. 2mol/LNaH2PO4 (pH7. 0)的流动相在0. 15mL/min的流速下等度洗脱,第二维反相色谱柱使用HypersilBDSC18 (35mm×4. ... 以GFC/RP模式构建全二维液相色谱系统,第一维凝胶过滤色谱柱使用ShodexProteinKW 802. 5(300mm×8mmi.d. ),以0. 2mol/LNaH2PO4 (pH7. 0)的流动相在0. 15mL/min的流速下等度洗脱,第二维反相色谱柱使用HypersilBDSC18 (35mm×4. 6mmi.d. ),在3mL/min的流速下梯度洗脱。采用平行柱交替分析的形式作切换接口, 2. 5min切换一次,两个反相柱交替富集、分析第一维洗脱产物。以5个标准蛋白混合物的分离评价该系统,在单独一维模式中不能分离的样品在全二维液相色谱中得到了较好的分离,二维系统的总峰容量为225。与一维色谱相比,系统的总峰容量、分辨率得到较大提高。并用于山羊血清的纯化分析,对一维分离中的重合谱峰进行验证,对制备纯化有一定的实际意义。 展开更多
关键词 山羊血清 分离 应用 液相色谱系统 模式构建 凝胶过滤 梯度洗脱 二维系统 实际意义 色谱柱 一维 GFC min 流动相 BDS 反相柱 混合物 维模式 分辨率 流速 切换 容量 纯化
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在线二维液相色谱技术在中药研究中的应用进展 被引量:24
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作者 高雯 宋慧鹏 +1 位作者 杨华 李萍 《色谱》 CAS CSCD 北大核心 2017年第1期121-128,共8页
中药的组成复杂,其化学成分的表征和识别一直是中药研究的基础和关键。在线二维液相色谱是基于两种分离模式构建的色谱分析技术,主要包括中心切割二维液相色谱和全二维液相色谱两种模式,因二者具有更高的峰容量而在中药研究中备受青睐... 中药的组成复杂,其化学成分的表征和识别一直是中药研究的基础和关键。在线二维液相色谱是基于两种分离模式构建的色谱分析技术,主要包括中心切割二维液相色谱和全二维液相色谱两种模式,因二者具有更高的峰容量而在中药研究中备受青睐。该文对在线二维液相色谱技术的概念和特点进行了讨论,并对二维液相色谱在中药研究中的应用进行了综述,以期为该技术在中药质量控制、物质基础表征、活性成分筛选等研究方面提供一定参考。 展开更多
关键词 全二维液相色谱 中心切割二维液相色谱 中药分析 活性成分筛选 综述
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全二维液相色谱串联质谱用于银杏叶提取物成分分析的研究 被引量:22
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作者 陈学国 孔亮 +2 位作者 盛亮洪 厉欣 邹汉法 《色谱》 CAS CSCD 北大核心 2005年第1期46-51,共6页
建立了全二维液相色谱串联质谱分离分析模式,将质脂体色谱柱和ODS反相色谱柱作为二维分析色谱柱,二者通过一个连有两个0 5mL定量环的八通阀耦联。质脂体色谱柱上的馏分在反相色谱柱上分离后,直接进入紫外 检测器,然后经分流器分流后进... 建立了全二维液相色谱串联质谱分离分析模式,将质脂体色谱柱和ODS反相色谱柱作为二维分析色谱柱,二者通过一个连有两个0 5mL定量环的八通阀耦联。质脂体色谱柱上的馏分在反相色谱柱上分离后,直接进入紫外 检测器,然后经分流器分流后进入大气压电离质谱。将该体系用于银杏叶提取物的组成研究,共检测到至少41个组分,结合紫外 可见光谱和质谱信息,其中13个组分初步鉴定为银杏内酯B、银杏内酯C、白果内酯、槲皮素芸香糖苷、槲皮素、槲皮素 3 O β D 葡萄糖基(1 2) α L 鼠李糖苷、槲皮素 3 O β D 葡萄糖苷、异鼠李素、山柰酚 3 O β D 芸香糖基(1 2) α L 鼠李糖苷、异鼠李素 3 O β D 芸香糖苷、山柰酚 3 O β D 葡萄糖苷、山柰酚和山柰酚 3 O β D 芸香糖苷。 展开更多
关键词 全二维液相色谱 质谱 银杏叶提取物 中药
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全二维液相色谱(IEC/RP)的构建与评价 被引量:8
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作者 王智聪 张庆合 +2 位作者 张维冰 李彤 赵中一 《高等学校化学学报》 SCIE EI CAS CSCD 北大核心 2005年第3期426-429,共4页
以 IEC/RP模式构建了二维液相色谱系统 ,采用平行交替柱捕集分析的 2位十通切换阀作接口 ,第一维洗脱产物按 1 0∶ 1的分流比分流后 ,得到 IEC和 RP切换谱图 .以 5个标准蛋白混合物的分离评价该系统 ,在单独一维模式中不能分离的样品在... 以 IEC/RP模式构建了二维液相色谱系统 ,采用平行交替柱捕集分析的 2位十通切换阀作接口 ,第一维洗脱产物按 1 0∶ 1的分流比分流后 ,得到 IEC和 RP切换谱图 .以 5个标准蛋白混合物的分离评价该系统 ,在单独一维模式中不能分离的样品在全二维液相色谱中得到了很好的分离 .二维系统的峰容量为 1 展开更多
关键词 全二维液相色谱 蛋白质 峰容量
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