[Objectives]To explore the methods for identifying pure honey.[Methods]Using 35 batches of Jiulongteng honey sourced from various production areas in Guangxi as the research subjects,this study investigated the chromo...[Objectives]To explore the methods for identifying pure honey.[Methods]Using 35 batches of Jiulongteng honey sourced from various production areas in Guangxi as the research subjects,this study investigated the chromogenic reactions of starch and dextrin,as well as the comparative study of thin-layer chromatography of oligosaccharides present in Jiulongteng honey.[Results]None of the 35 batches of Jiulongteng honey samples exhibited blue(indicating starch),green,or reddish-brown(indicating dextrin)coloration,suggesting that no adulterants such as artificially added starch,dextrin,or sugar were present in these samples.Furthermore,none of the 35 batches displayed additional spots below the corresponding positions of the control,indicating that the sugar composition was consistent with the oligosaccharide profile of natural honey.No components inconsistent with the oligosaccharide profile of natural honey were detected.Therefore,it can be concluded that the Jiulongteng honey samples in this experiment were pure and free from adulteration with starch,dextrin,or other sugar substances.[Conclusions]The method employed in this experiment is straightforward and quick to implement,effectively preventing adulterated honey from entering the market.It enhances the efficiency of quality control for Jiulongteng honey and promotes the healthy development of the Jiulongteng honey industry.展开更多
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
In this study,a high performance thin-layer chromatography/single quadrupole mass spectrometry QDa(HPTLC-QDa)method for robust authentication of Ganoderma lucidum,a popular and valuable herbal medicine,has been develo...In this study,a high performance thin-layer chromatography/single quadrupole mass spectrometry QDa(HPTLC-QDa)method for robust authentication of Ganoderma lucidum,a popular and valuable herbal medicine,has been developed.This method is simple and practical,which allows direct generation of characteristic mass spectra from the HPTLC plates automatically with the application of in situ solvent desorption interface.The HPTLC silica gel plates were developed with toluene-ethyl formate-formic acid(5:5:0.2,V/V)and all bands were transferred to QDa system directly in situ using 80%methanol with 0.1%formic acid as desorption solvent.The acquired HPTLC-QDa spectra showed that luminous yellow band b3,containing ganoderic acid B/G/H and ganodeneric acid B,the major active components of Ganoderma,could be found only in G.lucidum and G.lucidum(Antler-shaped),but not in G.sinense and G.applanatum.Moreover,bands b13 and b14 with m/z 475/477 and m/z 475/491/495,respectively,could be detected in G.lucidum(Antler-shaped),but not in G.lucidum,thus allowing simple and robust authentication of G.lucidum with confused species.This method is proved to be simple,practical and reproducible,which can be extended to analyze other herbal medicines.展开更多
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
The holistic characterization and quality control of all the medicinal herbs of proprietary Chinese medicines(PCMs)are of great significance to ensure their safety,efficacy,and consistency.Thin-layer chromatography(TL...The holistic characterization and quality control of all the medicinal herbs of proprietary Chinese medicines(PCMs)are of great significance to ensure their safety,efficacy,and consistency.Thin-layer chromatography(TLC),a simple and classic approach for qualitatively characterizing and examining quality markers of natural products,has been widely used in the characterization and quality control of traditional Chinese medicines.Zaoren Anshen(ZRAS)capsule,prepared from three medicinal herbs of fried Ziziphi Spinosae Semen,Salvia Miltiorrhiza Radix et Rhizoma,and vinegar-processed Schisandrae Chinensis Fructus,is a famous PCM in China for the treatment of insomnia,amnesia,and dizziness in clinical practice.However,no effective method is available so far for simultaneous identification and examination of all the three medicinal herbs of ZRAS capsule.In the present study,we developed a TLC method via twice-development and visualization by UV light or chromogenic agent,which could be used for simultaneous qualitative identification of all the three medicinal herbs of ZRAS capsule in one plate.Moreover,the sample preparation method was optimized.The developed TLC method was rapid,simple,low-cost,and effective,and thus it could be used for quality control of ZRAS capsule.展开更多
[Objectives] The aim was to determine the moisture,ash and extract contents in Leontopodium franchetii Beauv. from different localities. [Methods] The contents of moisture,total ash,acid-insoluble ash and extract in L...[Objectives] The aim was to determine the moisture,ash and extract contents in Leontopodium franchetii Beauv. from different localities. [Methods] The contents of moisture,total ash,acid-insoluble ash and extract in L. franchetii from different localities were determined according to the methods described in Chinese Pharmacopoeia( 2015 Edition). [Results] In the 10 samples,the contents of moisture were all less than or equal to 15. 0%; the contents of total ash were all below 12. 0%; and the contents of acid-insoluble ash were all less than 3. 0%. The contents of water-soluble extract( by cold-soaked extraction method) in the samples were all below 12. 0% except those from Hongyuan Prairie of Sichuan Province and Xinglong Mountain in Lanzhou City,Gansu Province. [Conclusions]The contents of the four indicators measured in this experiment varied by small margins,indicating that the quality was relatively stable. This study provides theoretical data for the revision of the quality standards for L. franchetii.展开更多
A newly designed quinazoline based compound, 6-pyridin-2-yl-5,6-dihydro-benzo[4,5]imidazo[1,2-c] quinazoline (PDBIQ) has shown the ability for the easy detection of nineteen amino acids on thin-layer chromatography pl...A newly designed quinazoline based compound, 6-pyridin-2-yl-5,6-dihydro-benzo[4,5]imidazo[1,2-c] quinazoline (PDBIQ) has shown the ability for the easy detection of nineteen amino acids on thin-layer chromatography plates as a spray reagent. This new reagent enabled to produce various distinguishable colors with amino acids with different RF values. The detection limits and the binding ability of PDBIQ with amino acids have been calculated. PDBIQ is also able to detect aminoacids from hydrolised seed protein. The title compound also exhibited profound inhibitory action against some gm (+ve) and gm (-ve) bacterial organisms. This paper deals with synthesis, spectroscopic application and biological evaluation of the organic moity.展开更多
Five phospholipids in human placenta were determined by phosphorus 31 nuclear magnetic resonance(^(31)P NMR)spectroscopy and thin-layer chromatography(TLC) scanning combined with the corrective method of absorbance pr...Five phospholipids in human placenta were determined by phosphorus 31 nuclear magnetic resonance(^(31)P NMR)spectroscopy and thin-layer chromatography(TLC) scanning combined with the corrective method of absorbance proportional coefficient. The NMR spectrometer used this investigation was a Bruker AM-500 spectrometer operating at 202.4 MHz for ^(31)P chemical shifts are relative to 85% phosphoric acid. TIC was carried out by silica gel H plate developed in chloroform-methanol-glacial acetic acid-ethanol-water(25:4:6:2:0.5),with Vaskovsky reagent as colour -developing agent of phospholipids.展开更多
采用顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)和液液萃取(liquid-liquid extraction,LLE)结合全二维气相色谱飞行时间质谱(comprehensive two-dimensional gas chromatography time of flight mass spectrometry...采用顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)和液液萃取(liquid-liquid extraction,LLE)结合全二维气相色谱飞行时间质谱(comprehensive two-dimensional gas chromatography time of flight mass spectrometry,GC×GC-TOF-MS)以及香气活度值(odour active value,OAV),对红星二锅头白酒的挥发性成分进行全面解析。研究发现,HS-SPME、LLE分别定性出928、802种挥发性化合物,共计定性出1304种挥发性化合物,共同定性出426种挥发性化合物。基于HS-SPME数据,通过香气数据库筛选出具有香气特征的382种香气化合物,其中酯类相对百分含量占比最高,其次是醇类、酸类和醛类。计算得到了49种香气化合物OAV>1,其中酯类(辛酸乙酯、异戊酸乙酯等)和萜烯类(β-大马酮)对白酒风味的贡献最大,醛类(异戊醛、己醛等)和含硫类(二甲基三硫)其次,醇类(1-辛烯-3-醇)和含氮类(2,3,5-三甲基吡嗪)也有一定风味贡献。该研究丰富了红星二锅头白酒的风味研究,也为下一步生产研究及调控提供了理论和数据支撑。展开更多
In this study, a system involving two-dimensional, column-switching high-performance liquid chromatography （HPLC） coupled with tandem mass spectrometry （LC-MS/MS） was developed and optimized for the analysis of an...In this study, a system involving two-dimensional, column-switching high-performance liquid chromatography （HPLC） coupled with tandem mass spectrometry （LC-MS/MS） was developed and optimized for the analysis of antibiotics and their related substances. In the first-dimensional chromatography, the analytes were separated on a zwitterion exchange-reversed phase-hydrophitic interaction （ZIC-RP-HILIC） mixed-mode column coupled with tandem mass spectrometry （LC-MS/MS）. A commonly used reversed phase LC column was employed in the second-dimensional chromatography. The mobile phase for the ZIC-RP-HILIC mixed-mode chromatography consisted of a volatile buffer that was compatible with LC-MS/MS, which enhanced the efficiency of ionization for structure elucidation. The antibiotic impurities eluted in the ion-pairing reversed phase chromatography were directly characterized by the ZIC-RP-HILIC-MS system, and the orthogonal separation of ZIC-RP-HILIC mixed-mode chromatography and reversed phase LC provided extra confidence that no impurity was missed. The efficiency of this method was demonstrated in the analysis of penicillin V potassium, oxacillin sodium, ceftriaxone sodium, and their impurities. In addition, this method is convenient for impurity profiling of antibiotics, and may be used for the analysis of other pharmaceutical ingredients.展开更多
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
The liquefied product of Salixpsammophila wood was separated by thin-layer chromatography （TLC） and column chromatography, and its structure was identified by nuclear magnetic resonance （NMR） spectra in our study....The liquefied product of Salixpsammophila wood was separated by thin-layer chromatography （TLC） and column chromatography, and its structure was identified by nuclear magnetic resonance （NMR） spectra in our study. The separation result indicates that the sample of liquefied S. psammophila contained at least two categories of components. The structure of the main components was guaiacyl C-1, C-2 of the hydroxyphenyl propane, i.e., the aromatic nucleus protons of lignin. Degradation and polycondensation reactions occurred when the S. psammophila wood was liquefied in phenol. Polycondensation reactions occurred among the depolymerization products from cellulose, the aromatic depolymerization products from lignin and the products of the displacement reactions between phenoxide ion and cellulose.展开更多
Liquid-liquid extraction-thin layer chromatography （LLE-TLC） has been a common and routine combined method for detection of drugs in biological materials. Solid-phase extraction （SPE） is gradually replacing the tr...Liquid-liquid extraction-thin layer chromatography （LLE-TLC） has been a common and routine combined method for detection of drugs in biological materials. Solid-phase extraction （SPE） is gradually replacing the tra- ditional LLE method. High performance thin layer chromatography （HPTLC） has several advantages over TLC. The present work studied the higher efficiency of a new SPE-HPTLC method over that of a routine LLE-TLC method, in extraction and detection of urinary morphine. Fifty-eight urine samples, primarily identified as mor- phine-positive samples by a strip test, ＇were re-screened by LLE-TLC and SPE-HPTLC. The results of LLE-TLC and SPE-HPTLC were then compared with each other. The results showed that the SPE-HPTLC detected 74% of total samples as morphine-positive samples whereas the LLE-TLC detected 48% of the same samples. We further discussed the effect of codeine abuse on TLC analysis of urinary morphine. Regarding the importance of morphine detection in urine, the present combined SPE-HPTLC method is suggested as a replacement method for detection of urinary morphine by many reference laboratories.展开更多
TongMai Granules is a Chinese medicine patent drug to treat cardiovascular diseases.It is prepared from the water extract of Dan-shen,Chuan-xiong and Ge-gen.The main compounds of TongMai Granules are isoflavone glycos...TongMai Granules is a Chinese medicine patent drug to treat cardiovascular diseases.It is prepared from the water extract of Dan-shen,Chuan-xiong and Ge-gen.The main compounds of TongMai Granules are isoflavone glycosides,isoflavones,and phenolic acids.However,it is difficult to detect low-polar compounds such as tanshinones and phthalides though they may also contribute to the therapeutic effect.In this work,an off-line two-dimensional chromatography method was developed to enrich the minor constituents in TongMai Granules.The extract was subjected to an SEP-PAK silica SPE column and eluted with petroleum ether,ethyl acetate–methanol(6:1,v/v),and methanol,successively.The three fractions were then analyzed using ultra-high performance liquid chromatography coupled with orbitrap mass spectrometry(UHPLC/orbitrap-MS).The isoflavones from Ge-gen,phenolic acids from Dan-shen and phthalides from Chuan-xiong were distributed in different fractions.A total of 131 compounds,including 59 from Ge-gen,26 from Dan-shen,43 from Chuan-xiong,and 3 common ones from Dan-shen and Chuan-xiong were tentatively identified.Among them,26 compounds were identified by comparing with reference standards.This study set a good example for comprehensive analysis of the constituents in traditional Chinese medicine formula.展开更多
Objective: To determine the thin-layer chromatography(TLC) fingerprint profiles and to evaluate the in vitro antioxidant activity of ethanol extracts of Muntingia calabura(M. calabura) leaves and stems.Methods: The le...Objective: To determine the thin-layer chromatography(TLC) fingerprint profiles and to evaluate the in vitro antioxidant activity of ethanol extracts of Muntingia calabura(M. calabura) leaves and stems.Methods: The leaves and stems were extracted using ethanol as solvent. The TLC separation of the phytochemical constituents of the leaf and ethanol extracts was carried out in ethyl acetate: n-hexane and chloroform: ethyl acetate mobile phase systems.Distinct spots were visualized under visible light, UV 254 nm, UV 366 nm and after spraying with vanillin-sulfuric acid. The 2,2-diphenyl-1-picrylhydrazyl free-radical scavenging assay was used to evaluate the antioxidant activity of the extracts.Results: Both the leaf and stem ethanol extracts at 4 mg/mL exhibited 2,2-diphenyl-1-picrylhydrazyl inhibition of more than 90%, relative to gallic acid. The results of TLC showed that the degree of resolution between the constituent spots was comparable between the two mobile phase systems using the different visualization wavelengths. Under the 254 nm visualization, few spots were observed in leaf and stem extracts. Visualization at 366 nm yielded the greatest number of observable spots of various colors in both leaf and stem extracts. More spots were visualized upon post-derivatization with vanillinsulfuric acid in the TLC chromatograms using chloroform: ethyl acetate mobile phase,compared to those in ethyl acetate: n-hexane mobile phase.Conclusions: M. calabura exhibited very high antioxidant activity in its leaves and stems ethanol extracts, both of which are used in traditional medicine. The TLC results demonstrated the presence of diverse secondary metabolites in the leaf and stem ethanol extracts, indicating that the antioxidant activity, including other bioactivities may be attributed to these phytochemical constituents. This paper has reported for the first time the TLC fingerprinting of M. calabura using visible light, UV 254 nm, UV 366 and postderivatization with vanillin-spray to visualize separate spots on TLC plates.展开更多
he use of an absorption trap off-line two-dimensional gas chromatography (2-DGC) in conjunction with a mass spectrometer greatly improved the separation andidefitification of minor constituents of a complex mixture su...he use of an absorption trap off-line two-dimensional gas chromatography (2-DGC) in conjunction with a mass spectrometer greatly improved the separation andidefitification of minor constituents of a complex mixture such as a natural essentialoil. The absorption trap device used as an interface of 2-DGC offered the advantageof convenient manipulation.展开更多
Aflatoxin B1 is a mycotoxin that can contaminate a wide feedstuffs variety. Ingestion of contaminated feed by poultry can lead to impaired health and zootechnical performances but also a human diet safety problem rela...Aflatoxin B1 is a mycotoxin that can contaminate a wide feedstuffs variety. Ingestion of contaminated feed by poultry can lead to impaired health and zootechnical performances but also a human diet safety problem related to residues presence in animal origin products. Aflatoxin B1 contamination of poultry feed samples marketed in Dakar city and in peri-urban areas (Gorom, Sangalkam) was studied. A total of 15 samples were collected from Dakar city markets as well as from poultry farms in Gorom and Sangalkam areas. Aflatoxin B1 quantification was performed by high performance liquid chromatography and thin-layer chromatography. HPLC results showed that all samples were contaminated with levels ranging from 0.15 to 22 ppb, 0.099 to 2.05 ppb and 0.099 to 4.95 ppb respectively for Gorom, Sangalkam and Dakar. Only the finishing feed from Gorom had an aflatoxin B1 level above the maximum limit set by regulations. TLC is a suitable method for aflatoxins detection. However, it was associated with overestimation for aflatoxin B1 quantification. Results suggest that poultry feed represents a real source of human diet contamination. In addition, HPLC remains the most reliable quantification technique for quality control.展开更多
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
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
Nucleoside is the main class of active components in Cordyceps sinensis. Thin-layer chromatography (TLC) is one of the most commonly used methods in pharmacopoeias for analyzing chemical components of herbal medicine....Nucleoside is the main class of active components in Cordyceps sinensis. Thin-layer chromatography (TLC) is one of the most commonly used methods in pharmacopoeias for analyzing chemical components of herbal medicine. Since the isocratic elution method cannot be applied successfully in TLC analysis for separating all the nucleoside components, the stepwise gradient elution has been developed in this work to separate eight nucleoside standards with success. In this way, quantitative analyses of the samples of Cordyceps sinensis were achieved via the pro-posed TLC procedure coupled with the scanning densitometric techniques of CAMAG and TLCQA methods for qualitative and quantitative analysis.展开更多
基金Supported by Enhancement Project of Basic Scientific Research Ability of Young and Middle-aged Teachers in Guangxi Universities(2020KY07040)School-level Scientific Research Project of Guangxi University of Chinese Medicine(2024QN022)Self-financed Scientific Research Project of Guangxi Zhuang Autonomous Region Administration of Traditional Chinese Medicine(GXZYL20240818).
文摘[Objectives]To explore the methods for identifying pure honey.[Methods]Using 35 batches of Jiulongteng honey sourced from various production areas in Guangxi as the research subjects,this study investigated the chromogenic reactions of starch and dextrin,as well as the comparative study of thin-layer chromatography of oligosaccharides present in Jiulongteng honey.[Results]None of the 35 batches of Jiulongteng honey samples exhibited blue(indicating starch),green,or reddish-brown(indicating dextrin)coloration,suggesting that no adulterants such as artificially added starch,dextrin,or sugar were present in these samples.Furthermore,none of the 35 batches displayed additional spots below the corresponding positions of the control,indicating that the sugar composition was consistent with the oligosaccharide profile of natural honey.No components inconsistent with the oligosaccharide profile of natural honey were detected.Therefore,it can be concluded that the Jiulongteng honey samples in this experiment were pure and free from adulteration with starch,dextrin,or other sugar substances.[Conclusions]The method employed in this experiment is straightforward and quick to implement,effectively preventing adulterated honey from entering the market.It enhances the efficiency of quality control for Jiulongteng honey and promotes the healthy development of the Jiulongteng honey industry.
基金the National Natural Science Foundation of China(Grant No.81872996)the State Key Research and Development Project(Grant No.2017YFC1702104)+1 种基金the State Key Project for the Creation of Major New Drugs(2018ZX09711001-009-010)the Tianjin Municipal Education Commission Research Project(Grant No.2017ZD07)。
文摘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.
基金National Key R&D Program of China(Nos.2019YFC1711000 and 2018YFC1707900)the National Natural Science Foundation of China(No.8200140730)Qi-Huang Scholar of National Traditional Chinese Medicine Leading Talents Support Program(2018)。
文摘In this study,a high performance thin-layer chromatography/single quadrupole mass spectrometry QDa(HPTLC-QDa)method for robust authentication of Ganoderma lucidum,a popular and valuable herbal medicine,has been developed.This method is simple and practical,which allows direct generation of characteristic mass spectra from the HPTLC plates automatically with the application of in situ solvent desorption interface.The HPTLC silica gel plates were developed with toluene-ethyl formate-formic acid(5:5:0.2,V/V)and all bands were transferred to QDa system directly in situ using 80%methanol with 0.1%formic acid as desorption solvent.The acquired HPTLC-QDa spectra showed that luminous yellow band b3,containing ganoderic acid B/G/H and ganodeneric acid B,the major active components of Ganoderma,could be found only in G.lucidum and G.lucidum(Antler-shaped),but not in G.sinense and G.applanatum.Moreover,bands b13 and b14 with m/z 475/477 and m/z 475/491/495,respectively,could be detected in G.lucidum(Antler-shaped),but not in G.lucidum,thus allowing simple and robust authentication of G.lucidum with confused species.This method is proved to be simple,practical and reproducible,which can be extended to analyze other herbal medicines.
基金supported by the National NaturalScience Foundation of China, No. 81200890
文摘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.
基金National Key Research and Development Program of China(Grant No.2018YFC1707300)。
文摘The holistic characterization and quality control of all the medicinal herbs of proprietary Chinese medicines(PCMs)are of great significance to ensure their safety,efficacy,and consistency.Thin-layer chromatography(TLC),a simple and classic approach for qualitatively characterizing and examining quality markers of natural products,has been widely used in the characterization and quality control of traditional Chinese medicines.Zaoren Anshen(ZRAS)capsule,prepared from three medicinal herbs of fried Ziziphi Spinosae Semen,Salvia Miltiorrhiza Radix et Rhizoma,and vinegar-processed Schisandrae Chinensis Fructus,is a famous PCM in China for the treatment of insomnia,amnesia,and dizziness in clinical practice.However,no effective method is available so far for simultaneous identification and examination of all the three medicinal herbs of ZRAS capsule.In the present study,we developed a TLC method via twice-development and visualization by UV light or chromogenic agent,which could be used for simultaneous qualitative identification of all the three medicinal herbs of ZRAS capsule in one plate.Moreover,the sample preparation method was optimized.The developed TLC method was rapid,simple,low-cost,and effective,and thus it could be used for quality control of ZRAS capsule.
基金Supported by National Key Technology Research and Development Program(2015BAC05B02)Fundamental Research Funds for the Central Universities(2018NZD10)
文摘[Objectives] The aim was to determine the moisture,ash and extract contents in Leontopodium franchetii Beauv. from different localities. [Methods] The contents of moisture,total ash,acid-insoluble ash and extract in L. franchetii from different localities were determined according to the methods described in Chinese Pharmacopoeia( 2015 Edition). [Results] In the 10 samples,the contents of moisture were all less than or equal to 15. 0%; the contents of total ash were all below 12. 0%; and the contents of acid-insoluble ash were all less than 3. 0%. The contents of water-soluble extract( by cold-soaked extraction method) in the samples were all below 12. 0% except those from Hongyuan Prairie of Sichuan Province and Xinglong Mountain in Lanzhou City,Gansu Province. [Conclusions]The contents of the four indicators measured in this experiment varied by small margins,indicating that the quality was relatively stable. This study provides theoretical data for the revision of the quality standards for L. franchetii.
文摘A newly designed quinazoline based compound, 6-pyridin-2-yl-5,6-dihydro-benzo[4,5]imidazo[1,2-c] quinazoline (PDBIQ) has shown the ability for the easy detection of nineteen amino acids on thin-layer chromatography plates as a spray reagent. This new reagent enabled to produce various distinguishable colors with amino acids with different RF values. The detection limits and the binding ability of PDBIQ with amino acids have been calculated. PDBIQ is also able to detect aminoacids from hydrolised seed protein. The title compound also exhibited profound inhibitory action against some gm (+ve) and gm (-ve) bacterial organisms. This paper deals with synthesis, spectroscopic application and biological evaluation of the organic moity.
文摘Five phospholipids in human placenta were determined by phosphorus 31 nuclear magnetic resonance(^(31)P NMR)spectroscopy and thin-layer chromatography(TLC) scanning combined with the corrective method of absorbance proportional coefficient. The NMR spectrometer used this investigation was a Bruker AM-500 spectrometer operating at 202.4 MHz for ^(31)P chemical shifts are relative to 85% phosphoric acid. TIC was carried out by silica gel H plate developed in chloroform-methanol-glacial acetic acid-ethanol-water(25:4:6:2:0.5),with Vaskovsky reagent as colour -developing agent of phospholipids.
文摘采用顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)和液液萃取(liquid-liquid extraction,LLE)结合全二维气相色谱飞行时间质谱(comprehensive two-dimensional gas chromatography time of flight mass spectrometry,GC×GC-TOF-MS)以及香气活度值(odour active value,OAV),对红星二锅头白酒的挥发性成分进行全面解析。研究发现,HS-SPME、LLE分别定性出928、802种挥发性化合物,共计定性出1304种挥发性化合物,共同定性出426种挥发性化合物。基于HS-SPME数据,通过香气数据库筛选出具有香气特征的382种香气化合物,其中酯类相对百分含量占比最高,其次是醇类、酸类和醛类。计算得到了49种香气化合物OAV>1,其中酯类(辛酸乙酯、异戊酸乙酯等)和萜烯类(β-大马酮)对白酒风味的贡献最大,醛类(异戊醛、己醛等)和含硫类(二甲基三硫)其次,醇类(1-辛烯-3-醇)和含氮类(2,3,5-三甲基吡嗪)也有一定风味贡献。该研究丰富了红星二锅头白酒的风味研究,也为下一步生产研究及调控提供了理论和数据支撑。
基金The Key Projects in the National Science&Technology Pillar Program during the Twelfth Five-year Plan Period(Grant No.2012BAK25B02)
文摘In this study, a system involving two-dimensional, column-switching high-performance liquid chromatography （HPLC） coupled with tandem mass spectrometry （LC-MS/MS） was developed and optimized for the analysis of antibiotics and their related substances. In the first-dimensional chromatography, the analytes were separated on a zwitterion exchange-reversed phase-hydrophitic interaction （ZIC-RP-HILIC） mixed-mode column coupled with tandem mass spectrometry （LC-MS/MS）. A commonly used reversed phase LC column was employed in the second-dimensional chromatography. The mobile phase for the ZIC-RP-HILIC mixed-mode chromatography consisted of a volatile buffer that was compatible with LC-MS/MS, which enhanced the efficiency of ionization for structure elucidation. The antibiotic impurities eluted in the ion-pairing reversed phase chromatography were directly characterized by the ZIC-RP-HILIC-MS system, and the orthogonal separation of ZIC-RP-HILIC mixed-mode chromatography and reversed phase LC provided extra confidence that no impurity was missed. The efficiency of this method was demonstrated in the analysis of penicillin V potassium, oxacillin sodium, ceftriaxone sodium, and their impurities. In addition, this method is convenient for impurity profiling of antibiotics, and may be used for the analysis of other pharmaceutical ingredients.
基金supported by the National Natural Science Foundation of China(No.30873196)Project of Modernization of Traditional Chinese Medicine of Shanghai(No.09dZ1975100)
文摘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.
基金supported by grants 200508010603 and 200711020504 from the key pro-ject of the Natural Science Foundation of the InnerMongolia Autonomous Region
文摘The liquefied product of Salixpsammophila wood was separated by thin-layer chromatography （TLC） and column chromatography, and its structure was identified by nuclear magnetic resonance （NMR） spectra in our study. The separation result indicates that the sample of liquefied S. psammophila contained at least two categories of components. The structure of the main components was guaiacyl C-1, C-2 of the hydroxyphenyl propane, i.e., the aromatic nucleus protons of lignin. Degradation and polycondensation reactions occurred when the S. psammophila wood was liquefied in phenol. Polycondensation reactions occurred among the depolymerization products from cellulose, the aromatic depolymerization products from lignin and the products of the displacement reactions between phenoxide ion and cellulose.
文摘Liquid-liquid extraction-thin layer chromatography （LLE-TLC） has been a common and routine combined method for detection of drugs in biological materials. Solid-phase extraction （SPE） is gradually replacing the tra- ditional LLE method. High performance thin layer chromatography （HPTLC） has several advantages over TLC. The present work studied the higher efficiency of a new SPE-HPTLC method over that of a routine LLE-TLC method, in extraction and detection of urinary morphine. Fifty-eight urine samples, primarily identified as mor- phine-positive samples by a strip test, ＇were re-screened by LLE-TLC and SPE-HPTLC. The results of LLE-TLC and SPE-HPTLC were then compared with each other. The results showed that the SPE-HPTLC detected 74% of total samples as morphine-positive samples whereas the LLE-TLC detected 48% of the same samples. We further discussed the effect of codeine abuse on TLC analysis of urinary morphine. Regarding the importance of morphine detection in urine, the present combined SPE-HPTLC method is suggested as a replacement method for detection of urinary morphine by many reference laboratories.
基金National Key Research and Development Program of China(Grant No.2018YFC1707301,2018YFC1707304)。
文摘TongMai Granules is a Chinese medicine patent drug to treat cardiovascular diseases.It is prepared from the water extract of Dan-shen,Chuan-xiong and Ge-gen.The main compounds of TongMai Granules are isoflavone glycosides,isoflavones,and phenolic acids.However,it is difficult to detect low-polar compounds such as tanshinones and phthalides though they may also contribute to the therapeutic effect.In this work,an off-line two-dimensional chromatography method was developed to enrich the minor constituents in TongMai Granules.The extract was subjected to an SEP-PAK silica SPE column and eluted with petroleum ether,ethyl acetate–methanol(6:1,v/v),and methanol,successively.The three fractions were then analyzed using ultra-high performance liquid chromatography coupled with orbitrap mass spectrometry(UHPLC/orbitrap-MS).The isoflavones from Ge-gen,phenolic acids from Dan-shen and phthalides from Chuan-xiong were distributed in different fractions.A total of 131 compounds,including 59 from Ge-gen,26 from Dan-shen,43 from Chuan-xiong,and 3 common ones from Dan-shen and Chuan-xiong were tentatively identified.Among them,26 compounds were identified by comparing with reference standards.This study set a good example for comprehensive analysis of the constituents in traditional Chinese medicine formula.
基金Supported by the Office of the Vice-Chancellor for Research and Development for the Outright Research Grant(Project No.151516 PNSE),the University of the Philippines Diliman
文摘Objective: To determine the thin-layer chromatography(TLC) fingerprint profiles and to evaluate the in vitro antioxidant activity of ethanol extracts of Muntingia calabura(M. calabura) leaves and stems.Methods: The leaves and stems were extracted using ethanol as solvent. The TLC separation of the phytochemical constituents of the leaf and ethanol extracts was carried out in ethyl acetate: n-hexane and chloroform: ethyl acetate mobile phase systems.Distinct spots were visualized under visible light, UV 254 nm, UV 366 nm and after spraying with vanillin-sulfuric acid. The 2,2-diphenyl-1-picrylhydrazyl free-radical scavenging assay was used to evaluate the antioxidant activity of the extracts.Results: Both the leaf and stem ethanol extracts at 4 mg/mL exhibited 2,2-diphenyl-1-picrylhydrazyl inhibition of more than 90%, relative to gallic acid. The results of TLC showed that the degree of resolution between the constituent spots was comparable between the two mobile phase systems using the different visualization wavelengths. Under the 254 nm visualization, few spots were observed in leaf and stem extracts. Visualization at 366 nm yielded the greatest number of observable spots of various colors in both leaf and stem extracts. More spots were visualized upon post-derivatization with vanillinsulfuric acid in the TLC chromatograms using chloroform: ethyl acetate mobile phase,compared to those in ethyl acetate: n-hexane mobile phase.Conclusions: M. calabura exhibited very high antioxidant activity in its leaves and stems ethanol extracts, both of which are used in traditional medicine. The TLC results demonstrated the presence of diverse secondary metabolites in the leaf and stem ethanol extracts, indicating that the antioxidant activity, including other bioactivities may be attributed to these phytochemical constituents. This paper has reported for the first time the TLC fingerprinting of M. calabura using visible light, UV 254 nm, UV 366 and postderivatization with vanillin-spray to visualize separate spots on TLC plates.
文摘he use of an absorption trap off-line two-dimensional gas chromatography (2-DGC) in conjunction with a mass spectrometer greatly improved the separation andidefitification of minor constituents of a complex mixture such as a natural essentialoil. The absorption trap device used as an interface of 2-DGC offered the advantageof convenient manipulation.
文摘Aflatoxin B1 is a mycotoxin that can contaminate a wide feedstuffs variety. Ingestion of contaminated feed by poultry can lead to impaired health and zootechnical performances but also a human diet safety problem related to residues presence in animal origin products. Aflatoxin B1 contamination of poultry feed samples marketed in Dakar city and in peri-urban areas (Gorom, Sangalkam) was studied. A total of 15 samples were collected from Dakar city markets as well as from poultry farms in Gorom and Sangalkam areas. Aflatoxin B1 quantification was performed by high performance liquid chromatography and thin-layer chromatography. HPLC results showed that all samples were contaminated with levels ranging from 0.15 to 22 ppb, 0.099 to 2.05 ppb and 0.099 to 4.95 ppb respectively for Gorom, Sangalkam and Dakar. Only the finishing feed from Gorom had an aflatoxin B1 level above the maximum limit set by regulations. TLC is a suitable method for aflatoxins detection. However, it was associated with overestimation for aflatoxin B1 quantification. Results suggest that poultry feed represents a real source of human diet contamination. In addition, HPLC remains the most reliable quantification technique for quality control.
基金sponsored by the Science and Technology Management Department of China National Petroleum Corporation
文摘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.
基金supported by the Science and Technology Management Department of China National Petroleum Corporation (Grant No. 2008A-0603)
文摘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.
基金the Research Committee of The Hong Kong Polytechnic University(No.G-V877)the Area of Excellence(AoE)of"Chinese Medicine Research and Further Development"of the University Grant Council(UGC)of Hong Kong Special Administrative Region(No.AoE/B-10/01)
文摘Nucleoside is the main class of active components in Cordyceps sinensis. Thin-layer chromatography (TLC) is one of the most commonly used methods in pharmacopoeias for analyzing chemical components of herbal medicine. Since the isocratic elution method cannot be applied successfully in TLC analysis for separating all the nucleoside components, the stepwise gradient elution has been developed in this work to separate eight nucleoside standards with success. In this way, quantitative analyses of the samples of Cordyceps sinensis were achieved via the pro-posed TLC procedure coupled with the scanning densitometric techniques of CAMAG and TLCQA methods for qualitative and quantitative analysis.
