A simple, sensible and reliable HPLC-DAD fingerprint analysis method for the raw materials of Oxytropisfalcata and Oxytropis chiliophylla, both of which were used as ＂Er-Da-Xia＂ in Tibetan medicines, was developed a...A simple, sensible and reliable HPLC-DAD fingerprint analysis method for the raw materials of Oxytropisfalcata and Oxytropis chiliophylla, both of which were used as ＂Er-Da-Xia＂ in Tibetan medicines, was developed and then subsequently applied to analyze samples collected from different locations or times. 19 common fingerprint peaks for O. falcata, 24 for O. chiliophylla, and 11 for the two herbs were designated respectively, including 7 identified characteristic peaks existing in both herbs and 1 uniquely presenting in O. chiliophylla. Although there were some slight differences in the chemicals of O. falcata and O. chiliophylla, the main components of both herbs were consistent generally. The results provided scientific basis, at least from the chemical point of view, for the reasonablity of two herbs being used as the same drug in Tibetan medicines and for the necessary of further investigation on their detailed chemical and pharmacological differences.展开更多
To facilitate the species identification and quality assessment of Chaihu （Bupleuri Radix）, a simple and valid chromatographic fingerprint method was developed. The method uses high-performance liquid chromatography...To facilitate the species identification and quality assessment of Chaihu （Bupleuri Radix）, a simple and valid chromatographic fingerprint method was developed. The method uses high-performance liquid chromatography coupled with evaporative light scattering detector （HPLC-ELSD） and the data analysis is assisted by professional analytical software recommended by the State Food and Drug Administration （SFDA）. The results indicate that Nan Chaihu raw materials and Chaihu decoction pieces vary markedly in chemical quality, while Bei Chaihu raw materials are relatively more stable. Furthermore, it is obvious that Nan Chaihu is chemically very different from Bei Chaihu, suggesting that Nan Chaihu may not be suitable for medicinal use. In addition, the obvious differences between the chromatograms of decoction pieces and raw materials, especially the peaks between 30 and 40 rain and after 45 rain, indicate possible effects of the processing procedures on the chemicals. By analyzing the fingerprints of all samples, 12 main saponin-like fingerprint peaks, of which at least three are characteristic peaks of saikosaponins a, c, and d, are proposed to be considered for further characterization and quality evaluation of Chaihu.展开更多
A study on relationship between molecular structure and chromatographic retention values for realizing the identification and prediction of chromatographic retention values has been the major task of chromatographic t...A study on relationship between molecular structure and chromatographic retention values for realizing the identification and prediction of chromatographic retention values has been the major task of chromatographic thermodynamics. In 1964, Prof. Lu Peizhang established the relationship between molecular structural parameters and chromatographic retention values in gas-liquid chromatography by using statistical thermodynamical methods. Based on his work, some Chinese researchers have performed the prediction of chromatographic retention values.展开更多
As an important branch of medicine, Traditional Chinese Medicine(TCM) has been applied for the treatment of diseases for thousands of years in China and other countries in East Asia. The Chinese Pharmacopoeia(ChP) is ...As an important branch of medicine, Traditional Chinese Medicine(TCM) has been applied for the treatment of diseases for thousands of years in China and other countries in East Asia. The Chinese Pharmacopoeia(ChP) is a drug code formulated by the Chinese government, and it includes a special volume for the monographs of TCM, which plays an important role in ensuring the quality of drugs. The use of quality control technology has always been a complex and important factor in TCM. Owing to the chemical diversity of TCM, chromatography technology has been proven to be a comprehensive strategy for the assessment of the overall quality of TCM and has become the main analytical method in the ChP.This article provides an overview of the classical and modern chromatographic technologies applied in the ChP, and summarizes the advantages and disadvantages of each technique in the TCM monographs.In 2020, the new edition of the Ch P(the 2020 edition) has been implemented at the end of 2020. This paper also contains a brief introduction about the application of chromatographic technologies in the new edition of the ChP.展开更多
Twenty eight alkyl(1-phenylsulfonyl) cycloalkane carboxylates were computed at the B3LYP/6-31G* level. Based on linear solvation energy theory, two quantitative correlation equations of the molecular structures of alk...Twenty eight alkyl(1-phenylsulfonyl) cycloalkane carboxylates were computed at the B3LYP/6-31G* level. Based on linear solvation energy theory, two quantitative correlation equations of the molecular structures of alkyl(1-phenylsulfonyl) cycloalkane carboxylate com- pounds to their chromatographic retention (capacity factor lgKW) and the toxicity for photo- bacterium phosphoreum (–lgEC50) were developed by using the molecular structural parameters as theoretical descriptors (r2 = 0.9501, 0.9488). The two quantitative correlation equations were consequently cross validated by leave-one-out (LOO) validation method with q2 of 0.9113 and 0.9281, respectively. The result showed that the two equations achieved in this work by B3LYP/6-31G* are both more advantageous than those from AM1, and can be used to predict the lgKW and –lgEC50 of congeneric organics.展开更多
An anion-exchange-based chromatographic separation approach was developed to selectively recover zinc and copper from the high-chlorine raffinate generated in the process of germanium chlorination distillation using 7...An anion-exchange-based chromatographic separation approach was developed to selectively recover zinc and copper from the high-chlorine raffinate generated in the process of germanium chlorination distillation using 717 resins based on the coordination difference between Zn^(2+)/Cu^(2+)and Cl^(-).The theoretical calculation and spectroscopic analyses suggested that the coordination between Zn^(2+)and Cl^(-)is much stronger than that between Cu^(2+)and Cl^(-),and the Cl-concentration significantly affects Zn(Ⅱ)and Cu(Ⅱ)species.The factors involving Cl-concentration,resin dosage,shaking speed,and temperature were investigated to determine the optimal condition,and the maximum separation factor of Zn/Cu reached as high as 479.2.The results of the adsorption isotherms,adsorption kinetics,SEM,FTIR,and XPS analyses indicated that the process followed the monolayer uniform chemisorption.Through the continuous adsorption experiments,Zn(Ⅱ)and Cu(Ⅱ)in the high-chlorine raffinate were separately recovered,allowing the reuse of residual waste acid and germanium.展开更多
Hydroxylated Polychlorinated Biphenyls （HO-PCBs） are the metabolite of polychlorinated biphenyls and have drawn much attention because they have hazard on human health and ecosystems. Molecular connectivity index ca...Hydroxylated Polychlorinated Biphenyls （HO-PCBs） are the metabolite of polychlorinated biphenyls and have drawn much attention because they have hazard on human health and ecosystems. Molecular connectivity index calculation has been performed for 19 HO-PCB compounds. A number of statistically based parameters have been extracted. Linear relationship between chromatographic retention index （RI） and the molecular connectivity index of 15 compounds in the training set has been established by multiple linear regression method. The other 4 HO-PCBs are used as the external test set. The result shows that the parameters can be well used to express the quantitative structure-retention relationship （QSRR） of HO-PCBs. Good stability and predictive ability have been demonstrated by leave-one-out cross-validation and the external test set.展开更多
The rhizome of Alpinia officinarum Hance is a well-known traditional Chinese medicine(TCM)and has been widely used for the remedy of gastrointestinal diseases.In the present study,a simple and rapid HPLC-DAD was devel...The rhizome of Alpinia officinarum Hance is a well-known traditional Chinese medicine(TCM)and has been widely used for the remedy of gastrointestinal diseases.In the present study,a simple and rapid HPLC-DAD was developed for the quality control of the rhizomes of A.officinarum.Its chemical fingerprint was established using raw material of 15 different origins in China.Similarity analysis(SA)and hierarchical clusting analysis(HCA)were applied to select the qualitative markers.Principal components analysis(PCA)was conducted to select the quantitative markers of the rhizomes of A.officinarum samples from different origins.The constituents were confirmed by(+)electrospray ionization LC-MS.12 constituents were selected as common peaks and 10 of them were confirmed by(+)electrospray ionization LC-MS.Six bioactive constituents including DPHA,galangin flavanone,galangin,galangin 3-methylether,DPHB and DPHC were simultaneous determination by using the HPLC-DAD analysis.The developed method was able to determine the bioactive components with excellent resolution,precision and recovery.The results indicated that chromatographic fingerprint combination with multi-components determination method is suitable for quality assessment of the rhizomes of A.officinarum.展开更多
A hydrophobic carbon dots(Glc-OCDs)derived from octadecylamine and glucose were successfully synthesized for the first time and then grafted onto the porous silica surface by the“Nano-on-Micro”strategy,which was ser...A hydrophobic carbon dots(Glc-OCDs)derived from octadecylamine and glucose were successfully synthesized for the first time and then grafted onto the porous silica surface by the“Nano-on-Micro”strategy,which was served as a new stationary phase(Sil-Glc-OCDs)for reversed-phase liquid chromatography.The structure of this stationary phase was carefully verified by laser scanning confocal microscope,Fourier transform infrared spectrometry,elemental analysis,contact angle measurement,etc.Several analytes including seven polycyclic aromatic hydrocarbons,eight alkylbenzenes,eight phenols and seven sulfonamides can be well separated on this stationary phase.Better separation performance for certain analytes over commercial C_(18) column was obtained.Interestingly,this stationary phase exhibited excellent chromatographic selectivity in the separation of the isomers of tert‑butylbenzene,sec‑butylbenzene,isobutylbenzene and n-butylbenzene.In addition,this new Sil-Glc-OCDs column was also applied for detection of calycosin-7-glucoside,ononin,calycosin,formononetin,genistein and isorhamnetin in the extract of Radix Astragali,which were found that the concentration was 0.15 g/L,0.088 g/L,0.14 g/L,0.086 g/L,0.18 g/L and 0.29 g/L,respectively.We believe that this CDs-grafted silica materials are promising for chromatographic separation.展开更多
Objective: To establish a new assay for platelet-activating factor (PAF), to compare it with bio-assay; and to discuss its significance in some elderly people diseases such as cerebral infarction and coronary heart di...Objective: To establish a new assay for platelet-activating factor (PAF), to compare it with bio-assay; and to discuss its significance in some elderly people diseases such as cerebral infarction and coronary heart disease. Methods: To measure PAF levels in 100 controls, 23 elderly patients with cerebral infarction and 65 cases with coronary heart disease by reversed phase high-performance liquid chromatographic technique (rHPLC). Results:rHPLC is more convenient, sensitive,specific, and less confusing, compared with bio-assay. The level of plasma PAF in patients with cerebral infarction was higher than that in the controls (P<0.01), and in patients with coronary heart disease. Conclusion: Detection of PAF with rHPLC is more reliable and more accurate. The new assay has important significance in PAF research.展开更多
The homochiral compounds play an important role in human health and pharmaceutical industry.Currently,the chromatographic enantioseparation has become one of the most effective and practical approach to obtain pure en...The homochiral compounds play an important role in human health and pharmaceutical industry.Currently,the chromatographic enantioseparation has become one of the most effective and practical approach to obtain pure enantiomers.Herein,the exploration of advanced materials,using as chromatographic chiral stationary phases for racemic separation,has attracted great attention.Thanks to their high enantioselectivity and controllable synthesis,the emerging chiral metal-organic frameworks (CMOFs)have been widely studied as the stationary phase in chromatographic technology.In this review,we will summarize the principles of synthetic strategies and mechanism of chiral microenvironment.In particular,the recent progress and research hotspot of CMOFs regarding as the chiral stationary phases in gas chromatography (GC),high-performance liquid chromatography (HPLC),and capillary electrochromatography (CEC),are elucidated systematically according to the published work.Last but not the least,we also highlight the challenges and perspectives of rational design of CMOFs,as well as their corresponding racemic separation.We envision that the review will provide a further understanding of CMOFs and facilitate the development of chromatographic enantioselective applications.展开更多
In this study, whole-oil gas chromatographic fingerprint analyses were performed on oils from the Es3^3 reservoir in the Liubei area of the Nanpu Sag. The gas chromatographic peaks of cyclic and branched alkanes with ...In this study, whole-oil gas chromatographic fingerprint analyses were performed on oils from the Es3^3 reservoir in the Liubei area of the Nanpu Sag. The gas chromatographic peaks of cyclic and branched alkanes with relatively high resolution from nCl0 to nC25 were selected to establish a database of whole-oil gas chromatographic peak height ratio fingerprints. Reservoir fluid connectivity was identified by using clustering analysis. This method can reflect the gas chromatography fingerprint information accurately and entirely, and avoid the one-sidedness of the star diagram method which only selects several fixed gas chromatographic peaks.展开更多
Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chro...Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chromatography/diode array detector(HPLC/DAD).The conditions of MAE were optimized by an orthogonal experiment,and then the authentication and validation of the chromatographic fingerprint were conducted.Nine peaks were identified as common peaks in the fingerprint chromatograms,and isofraxidin was considered as a reference compound and quantified.Relative standard deviations of retention time and peak area of each component were less than 3% and 8%,respectively.Similarity and difference analysis were conducted by use of PCA and relation coefficient.Twenty batches of sarcandra glabra(Thunb.)samples from two different producing areas could be classified into two different groups in the PCA model.The results showed that MAE-HPLC/DAD method was simple,efficient and stable for the study of complex chromatographic fingerprint of sarcandra glabra(Thunb.),which could provide more reliable and precise information for quality evaluation.展开更多
For quality control purpose,an approach of combining chromatographic fingerprint of Huaijiao pill（HP）and simultaneous determination of its major bioactive components was developed using high performance liquid chrom...For quality control purpose,an approach of combining chromatographic fingerprint of Huaijiao pill（HP）and simultaneous determination of its major bioactive components was developed using high performance liquid chromatography coupled with diode array detector（HPLC-DAD）.For fingerprint analysis,16 peaks were selected as the characteristic peaks to evaluate the similarities of different samples collected from different batches of three manufacturers.The similarities of 17 Huaijiao pill samples were beyond 0.966,indicating that samples from different batches and manufacturers were,to some extent,consistent.Additionally,simultaneous quantification of seven bioactive markers,namely sophoricoside,baicalin,naringin,genistein,rutin,quercetin and 5-O-methylvisammioside,in HP was performed to interpret the quality consistency.The validation of the proposed approach was acceptable,with the accuracy of 90.2%-106.9%in recovery test.The intra-day and inter-day precisions of the method were evaluated and the RSD values were less than 2.81%.The results from the quantitative data showed that the contents of six marker compounds（except for 5-O-methylvisammioside） were quite consistent between batches produced by one manufacturer and significantly distinctive among different manufacturers.The proposed approach was expected to be developed as a powerful tool for the quality control of HP.展开更多
Objective To facilitate the quality evaluation suitable for the unique characteristics of Chinese materia medica(CMM)by developing and implementing a novel approach known as the matching frequency statistical moment(M...Objective To facilitate the quality evaluation suitable for the unique characteristics of Chinese materia medica(CMM)by developing and implementing a novel approach known as the matching frequency statistical moment(MFSM)method.Methods This study established the MFSM method.To demonstrate its effectiveness,we applied this novel approach to analyze Danxi Granules(丹膝颗粒,DXG)and its constituent herbal materials.To begin with,the ultra-performance liquid chromatography(UPLC)was applied to obtain the chromatographic fingerprints of DXG and its constituent herbal materi-als.Next,the MFSM was leveraged to compress and integrate them into a new fingerprint with fewer analytical units.Then,we characterized the properties and variability of both the original and integrated fingerprints by calculating total quantum statistical moment(TQSM)parameters,information entropy and information amount,along with their relative standard deviation(RSD).Finally,we compared the TQSM parameters,information entropy and infor-mation amount,and their RSD between the traditional and novel fingerprints to validate the new analytical method.Results The chromatographic peaks of DXG and its 12 raw herbal materials were divided and integrated into peak families by the MFSM method.Before integration,the ranges of the peak number,three TQSM parameters,information entropy and information amount for each peak or peak family of UPLC fingerprints of DXG and its 12 raw herbal materials were 95.07−209.73,9390−183064μv·s,5.928−21.33 min,22.62−106.69 min^(2),4.230−6.539,and 50530−974186μv·s,respectively.After integration,the ranges of these parameters were 10.00−88.00,9390−183064μv·s,5.951−22.02 min,22.27−104.73 min^(2),2.223−5.277,and 38159−807200μv·s,respectively.Correspondingly,the RSD of all the aforementioned pa-rameters before integration were 2.12%−9.15%,6.04%−49.78%,1.15%−23.10%,3.97%−25.79%,1.49%−19.86%,and 6.64%−51.20%,respectively.However,after integration,they changed to 0.00%,6.04%−49.87%,1.73%−23.02%,3.84%−26.85%,1.17%−16.54%,and 6.40%−48.59%,respectively.The results demonstrated that in the newly integrated fingerprint,the analytical units of constituent herbal materials,information entropy and information amount were significantly reduced(P<0.05),while the TQSM parameters remained unchanged(P>0.05).Additionally,the RSD of the TQSM parameters,information entropy,and information amount didn’t show significant difference before and after integration(P>0.05),but the RSD of the number and area of the integrated analytical units significantly decreased(P<0.05).Conclusion The MFSM method could reduce the analytical units of constituent herbal mate-rials while maintain the properties and variability from their original fingerprint.Thus,it could serve as a feasible and reliable tool to reduce difficulties in analyzing multi-compo-nents within CMMs and facilitating the evaluation of their quality.展开更多
A sensor based on the technique of a piezoelectric quartz crystal microbalance (QCM) is analyzed for the detection of six organic volatile compounds with high olive oil sensory significance, such as hexanal, acetic ac...A sensor based on the technique of a piezoelectric quartz crystal microbalance (QCM) is analyzed for the detection of six organic volatile compounds with high olive oil sensory significance, such as hexanal, acetic acid, Z-3-hexenyl acetate, undecane, 1-octen-3-ol and 2-butanone. Four sample concentrations have been exposed to each QCM sensor constructed. The detection system is based on the sample adsorption on the forty sensing films coated at the surfaces of forty AT-cut gold-coated quartz crystals. Each sensing film has been prepared with different solution concentrations of ten materials, usually used as chromatographic sta-tionary phases. Sensing film coating process shows excellent repeatability, with coefficient values less than 0.50%. The frequency shifts of the piezoelectric crystals due to the adsorption of the volatile compounds have been measured as sensor responses, using a static measurement system. The results show that only five QCM sensors, with high sensitivity values, are enough to the detection of the volatile compounds studied. Therefore, the developed detection system presented herein provides a rapid identification of organic volatile compounds with elevated olive oil sensory connotation and it could be a substitute technique to the analytical methods normally used for the analysis of the olive oil flavor.展开更多
A counteracting chromatographic electrophoresis(CACE)separation device has been success-fully built and tested.Experiments are performed with protein mixtures of BSA,Hg,Mg and Cyto-cto study the separation performance...A counteracting chromatographic electrophoresis(CACE)separation device has been success-fully built and tested.Experiments are performed with protein mixtures of BSA,Hg,Mg and Cyto-cto study the separation performances,concentration profiles,start-up methodology as well as influ-ences of pH and ionic strength on the separation process.Mathematical models based on the fluiddynamics of the porous medium are proposed.Experiments indicate that the CACE process has agood commercial potential in protein engineering and fine chemicals purification.展开更多
High performance liquid chromatography-mass spectrometry is one of the most commonly used strategies for lipid analysis.The development of versatile chromatographic stationary phases to meet the increasing demands for...High performance liquid chromatography-mass spectrometry is one of the most commonly used strategies for lipid analysis.The development of versatile chromatographic stationary phases to meet the increasing demands for separation of complex lipids is very important.Styrene-maleic acid(SMA)copolymer is an amphiphilic polymer,which has been proven to have the ability to solubilize lipid molecules of various structures.In this study,styrene-maleic anhydride copolymer coated silica was first prepared by the thiol-ene click reaction.With L-cysteine hydrochloride or dodecanol as the post-modification reagents,Sil-SMA-amino acid and Sil-SMA-dodecanol stationary phase materials were further successfully fabricated via nucleophilic ring-opening reaction.The Fourier-transform infrared,thermogravimetric analysis,and elemental analysis results confirmed the two stationary phase materials were successfully prepared.Furthermore,both the Sil-SMA-dodecanol column and the Sil-SMA-amino acid column possessed reversed-phase/hydrophilic interaction/ion exchange mixed-mode retention mechanisms.The column efficiency of the Sil-SMA-derivatives columns reached 77,300 N/m.Based on the mixed-mode retention characteristics,the Sil-SMA-derivatives columns achieved both the lipid classes and species separation via a single column.The Sil-SMA-amino acid column was further successfully used to separate lipid extract from gastric cancer cell membrane.All these results demonstrated that the SMA-based stationary phase materials have a good potential for use in lipid separation.展开更多
A high-performance liquid chromatographic method using uv detection for thedetermination of 10 drugs of abuse is described. The method is sample and sensitive. The linear rangesare 20￣100ng/ml with relative standard ...A high-performance liquid chromatographic method using uv detection for thedetermination of 10 drugs of abuse is described. The method is sample and sensitive. The linear rangesare 20￣100ng/ml with relative standard deviations of 0.7 ￣ 2.6% (n=7) and detection limits of 5￣ 10ng/ml.展开更多
The cellulose tris (4-methylbenzoate) has been synthesised by the catalytic method and was supported at Gas Chrom Q. The absorption capability of cellulose tris (4-methylbenzoate) used as a gas chromatographic station...The cellulose tris (4-methylbenzoate) has been synthesised by the catalytic method and was supported at Gas Chrom Q. The absorption capability of cellulose tris (4-methylbenzoate) used as a gas chromatographic stationary phase was characterized by chromatographic method and the Clausius-Clapeyron equation. However, n-alcohols (C-1-C-8) were successfully separated on the column packed with Gas Chrom Q coated with cellullose tris (4-methylbenzoate).展开更多
基金National Natural Science Foundation of China (Grant No.21372015 and 20872006)
文摘A simple, sensible and reliable HPLC-DAD fingerprint analysis method for the raw materials of Oxytropisfalcata and Oxytropis chiliophylla, both of which were used as ＂Er-Da-Xia＂ in Tibetan medicines, was developed and then subsequently applied to analyze samples collected from different locations or times. 19 common fingerprint peaks for O. falcata, 24 for O. chiliophylla, and 11 for the two herbs were designated respectively, including 7 identified characteristic peaks existing in both herbs and 1 uniquely presenting in O. chiliophylla. Although there were some slight differences in the chemicals of O. falcata and O. chiliophylla, the main components of both herbs were consistent generally. The results provided scientific basis, at least from the chemical point of view, for the reasonablity of two herbs being used as the same drug in Tibetan medicines and for the necessary of further investigation on their detailed chemical and pharmacological differences.
基金The project of Quality Standards for Chinese Medicines and Information System Platform (Grant No.2009ZX09308004)National Natural Science Foundation of China (Grant No.21172008)
文摘To facilitate the species identification and quality assessment of Chaihu （Bupleuri Radix）, a simple and valid chromatographic fingerprint method was developed. The method uses high-performance liquid chromatography coupled with evaporative light scattering detector （HPLC-ELSD） and the data analysis is assisted by professional analytical software recommended by the State Food and Drug Administration （SFDA）. The results indicate that Nan Chaihu raw materials and Chaihu decoction pieces vary markedly in chemical quality, while Bei Chaihu raw materials are relatively more stable. Furthermore, it is obvious that Nan Chaihu is chemically very different from Bei Chaihu, suggesting that Nan Chaihu may not be suitable for medicinal use. In addition, the obvious differences between the chromatograms of decoction pieces and raw materials, especially the peaks between 30 and 40 rain and after 45 rain, indicate possible effects of the processing procedures on the chemicals. By analyzing the fingerprints of all samples, 12 main saponin-like fingerprint peaks, of which at least three are characteristic peaks of saikosaponins a, c, and d, are proposed to be considered for further characterization and quality evaluation of Chaihu.
基金present address: Dalian Institute of Chemical Physics, Dalian.
文摘A study on relationship between molecular structure and chromatographic retention values for realizing the identification and prediction of chromatographic retention values has been the major task of chromatographic thermodynamics. In 1964, Prof. Lu Peizhang established the relationship between molecular structural parameters and chromatographic retention values in gas-liquid chromatography by using statistical thermodynamical methods. Based on his work, some Chinese researchers have performed the prediction of chromatographic retention values.
文摘As an important branch of medicine, Traditional Chinese Medicine(TCM) has been applied for the treatment of diseases for thousands of years in China and other countries in East Asia. The Chinese Pharmacopoeia(ChP) is a drug code formulated by the Chinese government, and it includes a special volume for the monographs of TCM, which plays an important role in ensuring the quality of drugs. The use of quality control technology has always been a complex and important factor in TCM. Owing to the chemical diversity of TCM, chromatography technology has been proven to be a comprehensive strategy for the assessment of the overall quality of TCM and has become the main analytical method in the ChP.This article provides an overview of the classical and modern chromatographic technologies applied in the ChP, and summarizes the advantages and disadvantages of each technique in the TCM monographs.In 2020, the new edition of the Ch P(the 2020 edition) has been implemented at the end of 2020. This paper also contains a brief introduction about the application of chromatographic technologies in the new edition of the ChP.
基金This work was financially supported by the National Basic Research Program of China (2003CB415002), the China Postdoctoral Science Foundation (No. 2003033486) and the Natural Science Research Fund of University in Jiangsu (04KJB150149)
文摘Twenty eight alkyl(1-phenylsulfonyl) cycloalkane carboxylates were computed at the B3LYP/6-31G* level. Based on linear solvation energy theory, two quantitative correlation equations of the molecular structures of alkyl(1-phenylsulfonyl) cycloalkane carboxylate com- pounds to their chromatographic retention (capacity factor lgKW) and the toxicity for photo- bacterium phosphoreum (–lgEC50) were developed by using the molecular structural parameters as theoretical descriptors (r2 = 0.9501, 0.9488). The two quantitative correlation equations were consequently cross validated by leave-one-out (LOO) validation method with q2 of 0.9113 and 0.9281, respectively. The result showed that the two equations achieved in this work by B3LYP/6-31G* are both more advantageous than those from AM1, and can be used to predict the lgKW and –lgEC50 of congeneric organics.
基金financially supported by the Postdoctoral Research Foundation of Central South University,China(No.140050037)。
文摘An anion-exchange-based chromatographic separation approach was developed to selectively recover zinc and copper from the high-chlorine raffinate generated in the process of germanium chlorination distillation using 717 resins based on the coordination difference between Zn^(2+)/Cu^(2+)and Cl^(-).The theoretical calculation and spectroscopic analyses suggested that the coordination between Zn^(2+)and Cl^(-)is much stronger than that between Cu^(2+)and Cl^(-),and the Cl-concentration significantly affects Zn(Ⅱ)and Cu(Ⅱ)species.The factors involving Cl-concentration,resin dosage,shaking speed,and temperature were investigated to determine the optimal condition,and the maximum separation factor of Zn/Cu reached as high as 479.2.The results of the adsorption isotherms,adsorption kinetics,SEM,FTIR,and XPS analyses indicated that the process followed the monolayer uniform chemisorption.Through the continuous adsorption experiments,Zn(Ⅱ)and Cu(Ⅱ)in the high-chlorine raffinate were separately recovered,allowing the reuse of residual waste acid and germanium.
基金supported by the Natural Science Foundation of Zhejiang Province(No.LY12B07013 LY12C03009+1 种基金 Y5090304)State Key Laboratory of Environmental Chemistry and Ecotoxicology,Chinese Academy of Sciences(KF2011-19)
文摘Hydroxylated Polychlorinated Biphenyls （HO-PCBs） are the metabolite of polychlorinated biphenyls and have drawn much attention because they have hazard on human health and ecosystems. Molecular connectivity index calculation has been performed for 19 HO-PCB compounds. A number of statistically based parameters have been extracted. Linear relationship between chromatographic retention index （RI） and the molecular connectivity index of 15 compounds in the training set has been established by multiple linear regression method. The other 4 HO-PCBs are used as the external test set. The result shows that the parameters can be well used to express the quantitative structure-retention relationship （QSRR） of HO-PCBs. Good stability and predictive ability have been demonstrated by leave-one-out cross-validation and the external test set.
基金The National Natural Science Foundation of China(Grant No.81503210)the Medical Scientific Research Foundation of Guangdong Province(Grant No.B2017049)the Natural Science Foundation of Guangdong Food and Drug Vocational College(Grant No.2016YZ003)
文摘The rhizome of Alpinia officinarum Hance is a well-known traditional Chinese medicine(TCM)and has been widely used for the remedy of gastrointestinal diseases.In the present study,a simple and rapid HPLC-DAD was developed for the quality control of the rhizomes of A.officinarum.Its chemical fingerprint was established using raw material of 15 different origins in China.Similarity analysis(SA)and hierarchical clusting analysis(HCA)were applied to select the qualitative markers.Principal components analysis(PCA)was conducted to select the quantitative markers of the rhizomes of A.officinarum samples from different origins.The constituents were confirmed by(+)electrospray ionization LC-MS.12 constituents were selected as common peaks and 10 of them were confirmed by(+)electrospray ionization LC-MS.Six bioactive constituents including DPHA,galangin flavanone,galangin,galangin 3-methylether,DPHB and DPHC were simultaneous determination by using the HPLC-DAD analysis.The developed method was able to determine the bioactive components with excellent resolution,precision and recovery.The results indicated that chromatographic fingerprint combination with multi-components determination method is suitable for quality assessment of the rhizomes of A.officinarum.
基金financial support from Science and Technology Project of Science and Technology Bureau of Chengguan District in Lanzhou City(No.2020JSCX0033)National Natural Science Foundation of China(No.21822407)+1 种基金Youth Innovation Pro-motion Association CASthe National Research Foundation of Korea(NRF)grant funded by the Korean government(MSIT:Ministry of Science and ICT)(No.NRF-2019R1A2C1010032).
文摘A hydrophobic carbon dots(Glc-OCDs)derived from octadecylamine and glucose were successfully synthesized for the first time and then grafted onto the porous silica surface by the“Nano-on-Micro”strategy,which was served as a new stationary phase(Sil-Glc-OCDs)for reversed-phase liquid chromatography.The structure of this stationary phase was carefully verified by laser scanning confocal microscope,Fourier transform infrared spectrometry,elemental analysis,contact angle measurement,etc.Several analytes including seven polycyclic aromatic hydrocarbons,eight alkylbenzenes,eight phenols and seven sulfonamides can be well separated on this stationary phase.Better separation performance for certain analytes over commercial C_(18) column was obtained.Interestingly,this stationary phase exhibited excellent chromatographic selectivity in the separation of the isomers of tert‑butylbenzene,sec‑butylbenzene,isobutylbenzene and n-butylbenzene.In addition,this new Sil-Glc-OCDs column was also applied for detection of calycosin-7-glucoside,ononin,calycosin,formononetin,genistein and isorhamnetin in the extract of Radix Astragali,which were found that the concentration was 0.15 g/L,0.088 g/L,0.14 g/L,0.086 g/L,0.18 g/L and 0.29 g/L,respectively.We believe that this CDs-grafted silica materials are promising for chromatographic separation.
文摘Objective: To establish a new assay for platelet-activating factor (PAF), to compare it with bio-assay; and to discuss its significance in some elderly people diseases such as cerebral infarction and coronary heart disease. Methods: To measure PAF levels in 100 controls, 23 elderly patients with cerebral infarction and 65 cases with coronary heart disease by reversed phase high-performance liquid chromatographic technique (rHPLC). Results:rHPLC is more convenient, sensitive,specific, and less confusing, compared with bio-assay. The level of plasma PAF in patients with cerebral infarction was higher than that in the controls (P<0.01), and in patients with coronary heart disease. Conclusion: Detection of PAF with rHPLC is more reliable and more accurate. The new assay has important significance in PAF research.
基金supported by the Science and Technology Project of Education Department of Jiangxi Province (No.GJJ201249)。
文摘The homochiral compounds play an important role in human health and pharmaceutical industry.Currently,the chromatographic enantioseparation has become one of the most effective and practical approach to obtain pure enantiomers.Herein,the exploration of advanced materials,using as chromatographic chiral stationary phases for racemic separation,has attracted great attention.Thanks to their high enantioselectivity and controllable synthesis,the emerging chiral metal-organic frameworks (CMOFs)have been widely studied as the stationary phase in chromatographic technology.In this review,we will summarize the principles of synthetic strategies and mechanism of chiral microenvironment.In particular,the recent progress and research hotspot of CMOFs regarding as the chiral stationary phases in gas chromatography (GC),high-performance liquid chromatography (HPLC),and capillary electrochromatography (CEC),are elucidated systematically according to the published work.Last but not the least,we also highlight the challenges and perspectives of rational design of CMOFs,as well as their corresponding racemic separation.We envision that the review will provide a further understanding of CMOFs and facilitate the development of chromatographic enantioselective applications.
基金funded by Shandong Provincial Key Laboratory of Depositional Mineralization & Sedimentary Minerals (Project DMSM201009)Key Laboratory of Tectonics and Petroleum Resources (China University of Geosciences), Ministry of Education, China (Project TPR-2010-29)
文摘In this study, whole-oil gas chromatographic fingerprint analyses were performed on oils from the Es3^3 reservoir in the Liubei area of the Nanpu Sag. The gas chromatographic peaks of cyclic and branched alkanes with relatively high resolution from nCl0 to nC25 were selected to establish a database of whole-oil gas chromatographic peak height ratio fingerprints. Reservoir fluid connectivity was identified by using clustering analysis. This method can reflect the gas chromatography fingerprint information accurately and entirely, and avoid the one-sidedness of the star diagram method which only selects several fixed gas chromatographic peaks.
基金supported the National Natural Science Foundation of China(Nos.20375050 and 20905080)National Key Technologies R&D Program of the 11th-five-year Plan(No.2006BAK03A08)Guangdong Provincial Department of Science and Technology(No.2009B010900021)
文摘Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chromatography/diode array detector(HPLC/DAD).The conditions of MAE were optimized by an orthogonal experiment,and then the authentication and validation of the chromatographic fingerprint were conducted.Nine peaks were identified as common peaks in the fingerprint chromatograms,and isofraxidin was considered as a reference compound and quantified.Relative standard deviations of retention time and peak area of each component were less than 3% and 8%,respectively.Similarity and difference analysis were conducted by use of PCA and relation coefficient.Twenty batches of sarcandra glabra(Thunb.)samples from two different producing areas could be classified into two different groups in the PCA model.The results showed that MAE-HPLC/DAD method was simple,efficient and stable for the study of complex chromatographic fingerprint of sarcandra glabra(Thunb.),which could provide more reliable and precise information for quality evaluation.
文摘For quality control purpose,an approach of combining chromatographic fingerprint of Huaijiao pill（HP）and simultaneous determination of its major bioactive components was developed using high performance liquid chromatography coupled with diode array detector（HPLC-DAD）.For fingerprint analysis,16 peaks were selected as the characteristic peaks to evaluate the similarities of different samples collected from different batches of three manufacturers.The similarities of 17 Huaijiao pill samples were beyond 0.966,indicating that samples from different batches and manufacturers were,to some extent,consistent.Additionally,simultaneous quantification of seven bioactive markers,namely sophoricoside,baicalin,naringin,genistein,rutin,quercetin and 5-O-methylvisammioside,in HP was performed to interpret the quality consistency.The validation of the proposed approach was acceptable,with the accuracy of 90.2%-106.9%in recovery test.The intra-day and inter-day precisions of the method were evaluated and the RSD values were less than 2.81%.The results from the quantitative data showed that the contents of six marker compounds（except for 5-O-methylvisammioside） were quite consistent between batches produced by one manufacturer and significantly distinctive among different manufacturers.The proposed approach was expected to be developed as a powerful tool for the quality control of HP.
基金Natural Science Foundation of Hunan province(2022JJ30453 and 2024JJ6362)the Key Research and Development Program of Hunan Province(2022SK2014).
文摘Objective To facilitate the quality evaluation suitable for the unique characteristics of Chinese materia medica(CMM)by developing and implementing a novel approach known as the matching frequency statistical moment(MFSM)method.Methods This study established the MFSM method.To demonstrate its effectiveness,we applied this novel approach to analyze Danxi Granules(丹膝颗粒,DXG)and its constituent herbal materials.To begin with,the ultra-performance liquid chromatography(UPLC)was applied to obtain the chromatographic fingerprints of DXG and its constituent herbal materi-als.Next,the MFSM was leveraged to compress and integrate them into a new fingerprint with fewer analytical units.Then,we characterized the properties and variability of both the original and integrated fingerprints by calculating total quantum statistical moment(TQSM)parameters,information entropy and information amount,along with their relative standard deviation(RSD).Finally,we compared the TQSM parameters,information entropy and infor-mation amount,and their RSD between the traditional and novel fingerprints to validate the new analytical method.Results The chromatographic peaks of DXG and its 12 raw herbal materials were divided and integrated into peak families by the MFSM method.Before integration,the ranges of the peak number,three TQSM parameters,information entropy and information amount for each peak or peak family of UPLC fingerprints of DXG and its 12 raw herbal materials were 95.07−209.73,9390−183064μv·s,5.928−21.33 min,22.62−106.69 min^(2),4.230−6.539,and 50530−974186μv·s,respectively.After integration,the ranges of these parameters were 10.00−88.00,9390−183064μv·s,5.951−22.02 min,22.27−104.73 min^(2),2.223−5.277,and 38159−807200μv·s,respectively.Correspondingly,the RSD of all the aforementioned pa-rameters before integration were 2.12%−9.15%,6.04%−49.78%,1.15%−23.10%,3.97%−25.79%,1.49%−19.86%,and 6.64%−51.20%,respectively.However,after integration,they changed to 0.00%,6.04%−49.87%,1.73%−23.02%,3.84%−26.85%,1.17%−16.54%,and 6.40%−48.59%,respectively.The results demonstrated that in the newly integrated fingerprint,the analytical units of constituent herbal materials,information entropy and information amount were significantly reduced(P<0.05),while the TQSM parameters remained unchanged(P>0.05).Additionally,the RSD of the TQSM parameters,information entropy,and information amount didn’t show significant difference before and after integration(P>0.05),but the RSD of the number and area of the integrated analytical units significantly decreased(P<0.05).Conclusion The MFSM method could reduce the analytical units of constituent herbal mate-rials while maintain the properties and variability from their original fingerprint.Thus,it could serve as a feasible and reliable tool to reduce difficulties in analyzing multi-compo-nents within CMMs and facilitating the evaluation of their quality.
文摘A sensor based on the technique of a piezoelectric quartz crystal microbalance (QCM) is analyzed for the detection of six organic volatile compounds with high olive oil sensory significance, such as hexanal, acetic acid, Z-3-hexenyl acetate, undecane, 1-octen-3-ol and 2-butanone. Four sample concentrations have been exposed to each QCM sensor constructed. The detection system is based on the sample adsorption on the forty sensing films coated at the surfaces of forty AT-cut gold-coated quartz crystals. Each sensing film has been prepared with different solution concentrations of ten materials, usually used as chromatographic sta-tionary phases. Sensing film coating process shows excellent repeatability, with coefficient values less than 0.50%. The frequency shifts of the piezoelectric crystals due to the adsorption of the volatile compounds have been measured as sensor responses, using a static measurement system. The results show that only five QCM sensors, with high sensitivity values, are enough to the detection of the volatile compounds studied. Therefore, the developed detection system presented herein provides a rapid identification of organic volatile compounds with elevated olive oil sensory connotation and it could be a substitute technique to the analytical methods normally used for the analysis of the olive oil flavor.
基金Supported by National Natural Science Foundation of China
文摘A counteracting chromatographic electrophoresis(CACE)separation device has been success-fully built and tested.Experiments are performed with protein mixtures of BSA,Hg,Mg and Cyto-cto study the separation performances,concentration profiles,start-up methodology as well as influ-ences of pH and ionic strength on the separation process.Mathematical models based on the fluiddynamics of the porous medium are proposed.Experiments indicate that the CACE process has agood commercial potential in protein engineering and fine chemicals purification.
基金the financial support from National Natural Science Foundation of China(No.21675039)Natural Science Foundation of Hebei Province(Nos.B2019201327 and H2019201170)+1 种基金Hundred Outstanding Innovative Talents in Universities of Hebei Province(No.SLRC2019016)Young Talent of Hebei Province,Natural Science Interdisciplinary Research Program of Hebei University(No.DXK201912)。
文摘High performance liquid chromatography-mass spectrometry is one of the most commonly used strategies for lipid analysis.The development of versatile chromatographic stationary phases to meet the increasing demands for separation of complex lipids is very important.Styrene-maleic acid(SMA)copolymer is an amphiphilic polymer,which has been proven to have the ability to solubilize lipid molecules of various structures.In this study,styrene-maleic anhydride copolymer coated silica was first prepared by the thiol-ene click reaction.With L-cysteine hydrochloride or dodecanol as the post-modification reagents,Sil-SMA-amino acid and Sil-SMA-dodecanol stationary phase materials were further successfully fabricated via nucleophilic ring-opening reaction.The Fourier-transform infrared,thermogravimetric analysis,and elemental analysis results confirmed the two stationary phase materials were successfully prepared.Furthermore,both the Sil-SMA-dodecanol column and the Sil-SMA-amino acid column possessed reversed-phase/hydrophilic interaction/ion exchange mixed-mode retention mechanisms.The column efficiency of the Sil-SMA-derivatives columns reached 77,300 N/m.Based on the mixed-mode retention characteristics,the Sil-SMA-derivatives columns achieved both the lipid classes and species separation via a single column.The Sil-SMA-amino acid column was further successfully used to separate lipid extract from gastric cancer cell membrane.All these results demonstrated that the SMA-based stationary phase materials have a good potential for use in lipid separation.
文摘A high-performance liquid chromatographic method using uv detection for thedetermination of 10 drugs of abuse is described. The method is sample and sensitive. The linear rangesare 20￣100ng/ml with relative standard deviations of 0.7 ￣ 2.6% (n=7) and detection limits of 5￣ 10ng/ml.
文摘The cellulose tris (4-methylbenzoate) has been synthesised by the catalytic method and was supported at Gas Chrom Q. The absorption capability of cellulose tris (4-methylbenzoate) used as a gas chromatographic stationary phase was characterized by chromatographic method and the Clausius-Clapeyron equation. However, n-alcohols (C-1-C-8) were successfully separated on the column packed with Gas Chrom Q coated with cellullose tris (4-methylbenzoate).
