Since the chromatographic fingerprint was introduced, it has been accepted by many countries to assess the quality and authenticity of Chinese herbal medicine （CHM）. However, solely using the chromatographic fingerp...Since the chromatographic fingerprint was introduced, it has been accepted by many countries to assess the quality and authenticity of Chinese herbal medicine （CHM）. However, solely using the chromatographic fingerprint to assay numerous chemicals is not suitable for the assessment of the whole internal quality and pharmacodynamics of CHM. Consequently, it is necessary to develop a rational approach to connecting the chromatographic fingerprint with effective components to assess the internal quality of CHM. For this purpose, a spec^tun-effect relationship theory was proposed and accepted as a new method for the assessment of CHM because of its potential use to screen effective components from CHM. In this paper, we systematically reviewed the application of the spectrum-effect relationship theory in the research of CHM, including research mentality, different chromatographic analysis techniques, data processing technologies, and structure determination.展开更多
Amantadine （AMA） is an anti-viral drug used in apiculture to protect honeybee against the sacbrood virus （Morator aetatulae）. This study described a reliable high-performance liquid chromatographic （HPLC） method...Amantadine （AMA） is an anti-viral drug used in apiculture to protect honeybee against the sacbrood virus （Morator aetatulae）. This study described a reliable high-performance liquid chromatographic （HPLC） method for analyzing AMA in honey using a solid-phase extraction （SPE） cartridge （Plexa PCX） for purification, 4-fluoro-7- nitro-2,1,3-benzoxadiazole （NBD-F） as a pre-column derivatization agent, and fluorometric detection （λex =470 nm, λem=530 nm）. The chromatographic separation was performed on an XDB C18 column （150×4.6 mm i.d.） using 0.1% trifluoroacetic acid/acetonitrile （35 ; 65, V/V） as the mobile phase at a flow rate of 1.0 mLomin 1 with a run time of 20 min. Under these optimal conditions, a linear relationship was observed in the range of 0.025--1.0μg·mL-1 with a good correlation coefficient （0.998） and low limit of detection （0.0080 μg·g-1）, the recoveries were all above 90%, and the intra-day and inter-day precision （RSD） ranged from 3.4%--5.1%.展开更多
Understanding hydrocarbon migration and accumulation mechanisms is one of the key scientif ic problems that should be solved for effective hydrocarbon exploration in the superimposed basins developed in northwest Chin...Understanding hydrocarbon migration and accumulation mechanisms is one of the key scientif ic problems that should be solved for effective hydrocarbon exploration in the superimposed basins developed in northwest China. The northwest striking No.1 slope break zone, which is a representative of superimposed basins in the Tarim Basin, can be divided into five parts due to the intersection of the northeast strike-slip faults. Controlled by the tectonic framework, the types and properties of reservoirs and the hydrocarbon compositions can also be divided into five parts from east to west. Anomalies of all the parameters were found on the fault intersection zone and weakened up-dip along the structural ridge away from it. Thus, it can be inferred that the intersection zone is the hydrocarbon charging position. This new conclusion differs greatly from the traditional viewpoint, which believes that the hydrocarbon migrates and accumulates along the whole plane of the No.1 slope break zone. The viewpoint is further supported by the evidence from the theory of main pathway systems, obvious improvement of the reservoir quality （2-3 orders of magnitude at the intersection zone） and the formation mechanisms of the fault intersection zone. Differential hydrocarbon migration and entrapment exists in and around the strike- slip faults. This is controlled by the internal structure of faults. It is concluded that the more complicated the fault structure is, the more significant the effects will be. If there is a deformation band, it will hinder the cross fault migration due to the common feature of two to four orders of magnitude reduction in permeability. Otherwise, hydrocarbons tend to accumulate in the up-dip structure under the control of buoyancy. Further research on the internal fault structure should be emphasized.展开更多
AIM: To develop and validate a high performance liquid chromatography(HPLC) coupled with diode array and evaporative light scattering detectors(DAD-ELSD) method for the quantitative determination and fingerprint analy...AIM: To develop and validate a high performance liquid chromatography(HPLC) coupled with diode array and evaporative light scattering detectors(DAD-ELSD) method for the quantitative determination and fingerprint analysis of ten active constituents in three chemical classes(namely, xanthone glycosides, steroidal saponins, and alkaloids) in Zhimu-Huangbai herb pair(ZB). METHOD: Chromatographic separation was performed on a Diamonsil C18 column(4.6 mm × 250 mm, 5 μm, Dikma) by gradient elution using acetic acid in acetonitrile solution at a flow rate of 1.0 mL·min–1 at 260 nm. The drift tube temperature of ELSD was set to 60 ℃ and nebulizer gas pressure was 4.0 Bar. Method validation was performed to assure its linearity, limits of detection and quantification, precision, repeatability, stability, and accuracy. RESULTS: The HPLC-DAD-ELSD method allowed the quantification of ten compounds(phellodendrine, jatrorrhizine, palmatine, berberine, neomangiferin, mangiferin, timosaponin E-I, timosaponin B-II, timosaponin B, and timosaponin A-III), and was successfully applied to fingerprint analysis for ten batches of ZB samples. CONCLUSION: This was the first time to apply the combination of DAD and ELSD for the simultaneous determination of ten active ingredients in ZB. The results showed that the combination of quantitative analysis for marker ingredients and chemical fingerprint for the TCM herb pair provides a potentially powerful, widely introduced, and internationally accepted strategy for assessment of complex TCM formulas.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 HPLC method for routine quality control of biapenem was established. A Dikma Diamonsil Cls column （250 mm× 4.6 mm, 5 μm） was used with diode array detection and single wavelength detection at 220 mm. The mo...An HPLC method for routine quality control of biapenem was established. A Dikma Diamonsil Cls column （250 mm× 4.6 mm, 5 μm） was used with diode array detection and single wavelength detection at 220 mm. The mobile phase was consisted of acetonitrile-0 1% triethylamine water （1：99, v/v）. The liner range for biapenem quantification was 0.05-10.0 mg/mL （r2- 0.999）. The LOD and LOQ of impurity were 4.8 ng （S/N 3） and 18.5 ng （S/N = 10）, respectively. Intra-day RSD of main impurity and total impurity were 1.84% and 3.37% （n = 3）; inter-day RSD of main impurity and total impurity were 4.84% and 7.58% （n = 9）. The test solution was stable when stored at 4 ℃ for 6 h. The impurity peaks of biapenem can be identified by chromatographic spectral correlation analysis using high-performance liquid chromatography~tiode array detection data from the quality control method by calculating correlation coefficients without reference standards. Two hydrolysis degradation products with relative retention times （RRTs） of 0.528 and 0.743, two dimers with RRTs of 1.062 and 2.817 were identified in the quality control chromatogram. It provides a new way to identify impurity peaks by the routine HPLC-UV method.展开更多
哺乳动物的尿液挥发性成分被认为是同哺乳动物信息激素一样重要的物质,迄今报道的野生动物尿液挥发性成分研究的有狮（Panthera leo）（Andersen and Vulpius,1999）、山猫（Lynx rufus）（Mattina et al.,1991）、土狼（Canis lupus）...哺乳动物的尿液挥发性成分被认为是同哺乳动物信息激素一样重要的物质,迄今报道的野生动物尿液挥发性成分研究的有狮（Panthera leo）（Andersen and Vulpius,1999）、山猫（Lynx rufus）（Mattina et al.,1991）、土狼（Canis lupus）（Raymer et al.,1986）、郊狼（Canis latrans）（Schultz,1988）、展开更多
This paper described the principle of digitized chromatographic fingerprint spectrum and established digitized chromatographic fingerprint spectra of ten brands of Chinese famous tea by the micellar electrokinetic chr...This paper described the principle of digitized chromatographic fingerprint spectrum and established digitized chromatographic fingerprint spectra of ten brands of Chinese famous tea by the micellar electrokinetic chromatography. This work was done using a 25 mmol·L -1 sodium dodecylsulfate in a 20 mmol·L -1 borate (pH 7 0) solution as running buffer, 20 kV applied potential and detection at 280 nm. The chromatographic fingerprint spectra were digitized by the relative retention value ( α ) and the relative area ( S r), and were analyzed to identify the tea samples. In the absence of the standard samples, the present method was easy setup and inexpensive, and provided the applicable information for the quality assessment of teas.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
基金supported by Ministry of Education Research Fund for the Doctoral Program(20130013120001 and 20120013130002)Beijing University of Chinese Medicine Young Teachers of Special Autonomy Issue(2013-QNJSZX008)Beijing University of Chinese Medicine Scientific Research Innovation Team(2011-CXTD-014)
文摘Since the chromatographic fingerprint was introduced, it has been accepted by many countries to assess the quality and authenticity of Chinese herbal medicine （CHM）. However, solely using the chromatographic fingerprint to assay numerous chemicals is not suitable for the assessment of the whole internal quality and pharmacodynamics of CHM. Consequently, it is necessary to develop a rational approach to connecting the chromatographic fingerprint with effective components to assess the internal quality of CHM. For this purpose, a spec^tun-effect relationship theory was proposed and accepted as a new method for the assessment of CHM because of its potential use to screen effective components from CHM. In this paper, we systematically reviewed the application of the spectrum-effect relationship theory in the research of CHM, including research mentality, different chromatographic analysis techniques, data processing technologies, and structure determination.
文摘Amantadine （AMA） is an anti-viral drug used in apiculture to protect honeybee against the sacbrood virus （Morator aetatulae）. This study described a reliable high-performance liquid chromatographic （HPLC） method for analyzing AMA in honey using a solid-phase extraction （SPE） cartridge （Plexa PCX） for purification, 4-fluoro-7- nitro-2,1,3-benzoxadiazole （NBD-F） as a pre-column derivatization agent, and fluorometric detection （λex =470 nm, λem=530 nm）. The chromatographic separation was performed on an XDB C18 column （150×4.6 mm i.d.） using 0.1% trifluoroacetic acid/acetonitrile （35 ; 65, V/V） as the mobile phase at a flow rate of 1.0 mLomin 1 with a run time of 20 min. Under these optimal conditions, a linear relationship was observed in the range of 0.025--1.0μg·mL-1 with a good correlation coefficient （0.998） and low limit of detection （0.0080 μg·g-1）, the recoveries were all above 90%, and the intra-day and inter-day precision （RSD） ranged from 3.4%--5.1%.
基金supported by the National 973 Basic Research Program (Grant No.2006CB202308)the Major National Science & Technology Program (2008ZX05008-004-012)
文摘Understanding hydrocarbon migration and accumulation mechanisms is one of the key scientif ic problems that should be solved for effective hydrocarbon exploration in the superimposed basins developed in northwest China. The northwest striking No.1 slope break zone, which is a representative of superimposed basins in the Tarim Basin, can be divided into five parts due to the intersection of the northeast strike-slip faults. Controlled by the tectonic framework, the types and properties of reservoirs and the hydrocarbon compositions can also be divided into five parts from east to west. Anomalies of all the parameters were found on the fault intersection zone and weakened up-dip along the structural ridge away from it. Thus, it can be inferred that the intersection zone is the hydrocarbon charging position. This new conclusion differs greatly from the traditional viewpoint, which believes that the hydrocarbon migrates and accumulates along the whole plane of the No.1 slope break zone. The viewpoint is further supported by the evidence from the theory of main pathway systems, obvious improvement of the reservoir quality （2-3 orders of magnitude at the intersection zone） and the formation mechanisms of the fault intersection zone. Differential hydrocarbon migration and entrapment exists in and around the strike- slip faults. This is controlled by the internal structure of faults. It is concluded that the more complicated the fault structure is, the more significant the effects will be. If there is a deformation band, it will hinder the cross fault migration due to the common feature of two to four orders of magnitude reduction in permeability. Otherwise, hydrocarbons tend to accumulate in the up-dip structure under the control of buoyancy. Further research on the internal fault structure should be emphasized.
基金supported by the Natural Science Foundation of Shanghai City,China(No.10411969800)the National Nature Science Foundation of China(Nos.81202866 and 81302856)
文摘AIM: To develop and validate a high performance liquid chromatography(HPLC) coupled with diode array and evaporative light scattering detectors(DAD-ELSD) method for the quantitative determination and fingerprint analysis of ten active constituents in three chemical classes(namely, xanthone glycosides, steroidal saponins, and alkaloids) in Zhimu-Huangbai herb pair(ZB). METHOD: Chromatographic separation was performed on a Diamonsil C18 column(4.6 mm × 250 mm, 5 μm, Dikma) by gradient elution using acetic acid in acetonitrile solution at a flow rate of 1.0 mL·min–1 at 260 nm. The drift tube temperature of ELSD was set to 60 ℃ and nebulizer gas pressure was 4.0 Bar. Method validation was performed to assure its linearity, limits of detection and quantification, precision, repeatability, stability, and accuracy. RESULTS: The HPLC-DAD-ELSD method allowed the quantification of ten compounds(phellodendrine, jatrorrhizine, palmatine, berberine, neomangiferin, mangiferin, timosaponin E-I, timosaponin B-II, timosaponin B, and timosaponin A-III), and was successfully applied to fingerprint analysis for ten batches of ZB samples. CONCLUSION: This was the first time to apply the combination of DAD and ELSD for the simultaneous determination of ten active ingredients in ZB. The results showed that the combination of quantitative analysis for marker ingredients and chemical fingerprint for the TCM herb pair provides a potentially powerful, widely introduced, and internationally accepted strategy for assessment of complex TCM formulas.
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Foundation item： National Key New Drag R＆D Program Foundation of China （Grant No. 2009ZX09313-027）.
文摘An HPLC method for routine quality control of biapenem was established. A Dikma Diamonsil Cls column （250 mm× 4.6 mm, 5 μm） was used with diode array detection and single wavelength detection at 220 mm. The mobile phase was consisted of acetonitrile-0 1% triethylamine water （1：99, v/v）. The liner range for biapenem quantification was 0.05-10.0 mg/mL （r2- 0.999）. The LOD and LOQ of impurity were 4.8 ng （S/N 3） and 18.5 ng （S/N = 10）, respectively. Intra-day RSD of main impurity and total impurity were 1.84% and 3.37% （n = 3）; inter-day RSD of main impurity and total impurity were 4.84% and 7.58% （n = 9）. The test solution was stable when stored at 4 ℃ for 6 h. The impurity peaks of biapenem can be identified by chromatographic spectral correlation analysis using high-performance liquid chromatography~tiode array detection data from the quality control method by calculating correlation coefficients without reference standards. Two hydrolysis degradation products with relative retention times （RRTs） of 0.528 and 0.743, two dimers with RRTs of 1.062 and 2.817 were identified in the quality control chromatogram. It provides a new way to identify impurity peaks by the routine HPLC-UV method.
文摘哺乳动物的尿液挥发性成分被认为是同哺乳动物信息激素一样重要的物质,迄今报道的野生动物尿液挥发性成分研究的有狮（Panthera leo）（Andersen and Vulpius,1999）、山猫（Lynx rufus）（Mattina et al.,1991）、土狼（Canis lupus）（Raymer et al.,1986）、郊狼（Canis latrans）（Schultz,1988）、
文摘This paper described the principle of digitized chromatographic fingerprint spectrum and established digitized chromatographic fingerprint spectra of ten brands of Chinese famous tea by the micellar electrokinetic chromatography. This work was done using a 25 mmol·L -1 sodium dodecylsulfate in a 20 mmol·L -1 borate (pH 7 0) solution as running buffer, 20 kV applied potential and detection at 280 nm. The chromatographic fingerprint spectra were digitized by the relative retention value ( α ) and the relative area ( S r), and were analyzed to identify the tea samples. In the absence of the standard samples, the present method was easy setup and inexpensive, and provided the applicable information for the quality assessment of teas.
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.
