Objective: To compare the pharmacokinetic differences of the main components of Naoxintong capsule(NXTC) in normal and acute blood stasis rats. Materials and Methods: Rats were subcutaneously injected with adrenaline ...Objective: To compare the pharmacokinetic differences of the main components of Naoxintong capsule(NXTC) in normal and acute blood stasis rats. Materials and Methods: Rats were subcutaneously injected with adrenaline hydrochloride twice;during the two subcutaneous injections, the rats were placed in ice water for 4 min to reproduce the model rat of acute blood stasis. The normal and acute blood stasis rats were administrated a 5.04 g/kg dose of NXTC suspension. Then, blood samples were collected from the posterior retinal venous plexus at different time points. Plasma concentrations of four major bio-active components including caffeic acid, ferulic acid, formononetin, and tanshinone IIA in NXTC were measured using ultra-performance liquid chromatography coupled with triple-quadrupole mass spectrometry. Phoenix Win Nonlin v6.2 software was used to calculate the pharmacokinetic parameters. Results: Compared with the normal rats, the acute blood stasis rats showed a significant decrease in C_(max) of ferulic acid and formononetin, AUC_(all) of caffeic acid and ferulic acid, and AUC_(INF_obs) of ferulic acid. Conversely, an increase in the Vz_F_obs and MRT_(last) of ferulic acid and caffeic acid was observed. These findings demonstrate that the absorption of the four NXTC components was weakened in the acute blood stasis rats and that the elimination time was prolonged. Conclusions: The significant difference in some parameters of the four NXTC components between the normal and acute blood stasis rats might be caused by an increase in blood viscosity and the subsequent slowing down of blood flow in the acute blood stasis rats. The pharmacokinetic study conducted in pathological state can provide important information and scientific basis for further rational clinical application of NXTC.展开更多
Objective:There are different geographic origins of Aconiti Kusnezoffii Radixs(AKRs)sold in the market with different quality.This study aims to establish a rapid analysis method to distinguish the different geographi...Objective:There are different geographic origins of Aconiti Kusnezoffii Radixs(AKRs)sold in the market with different quality.This study aims to establish a rapid analysis method to distinguish the different geographic origins of AKRs and to realize the rapid evaluation of their quality.Methods:An ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry(UPLC-Q-TOF MS)method was utilized to acquire the constituents'information of AKRs from different geographic origins.MSE data and Progenesis QI software were employed to identify the chemical constitutes.Principal component analysis(PCA)was applied to comparing MS data to find the chemical markers of AKRs from different geographic origins.Results:Twenty-three components were detected and 17 out of them were identified,including diester-diterpenoid alkaloids,monoester-diterpenoid alkaloids,and amine-diterpenoid alkaloids.Three pairs of isomers were detected and two of them were distinguished by the retention time of standard samples.Thirteen chemical markers were screened out through PCA and orthogonal partial least square discriminant analysis.Through detecting Napelline or isomer of Napelline(m/z 360.2530)and Aconifine(m/z 662.3170),AKRs from inner Mongolia autonomous could be screened.According to the existence of benzoylaconine(m/z 604.3108)and Indaconitine(m/z 630.3159),it could be confirmed that the AKRs are from Xinjiang Uygur autonomous.AKRs that cannot detect compounds above-mentioned could be from Liaoning or Shanxi Province.Conclusions:The chemical profile could be used not only to distinguish the AKRs from different geographic origins but also to identify the true and false of AKRs.This study lays a foundation for the study of efficacy and toxic of AKRs.展开更多
A rapid and high selective ultra-performance liquid chromatography(UPLC)with tandem mass spectrometry method for simultaneous determination of six compounds including albiflorin,paeoniflorin,picroside I,picroside II,s...A rapid and high selective ultra-performance liquid chromatography(UPLC)with tandem mass spectrometry method for simultaneous determination of six compounds including albiflorin,paeoniflorin,picroside I,picroside II,saikosaponin A,and saikosaponin D in rat plasma was developed and validated using butyl p-hydroxybenzoate as an internal standard.One-step direct protein precipitation with acetonitrile was used to extract the compounds from the rat plasma samples.Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7μm)at a flow rate of 0.4 m L/min,using gradient mode containing 0.1%formic acid in water and acetonitrile were used as the Mobile phase A and B.Electrospray ionization in negative ion mode and multiple reaction monitoring were used to identify and quantify active components.Calibration curves showed good linearity(R^2>0.9908)over a wide concentration range for all compounds.The intra-and interday precision(relative standard deviation)ranged 2.4%–7.0%and 2.6%–8.0%,respectively.The accuracy(relative error)was from-13.0%to 13.2%at all quality control levels.The recovery ranged from 81.1%to 92.5%.The validated method was successfully applied to pharmacokinetic study in rats after oral administration of Qing Gan-Shu Yu-Fang.The results show that one can draw a conclusion that these six active ingredients can be quickly absorbed and play a pharmacodynamic role rapidly in vivo.展开更多
Objective: Granules of herbal extracts are a popular medicinal preparation consumed in traditional Chinese medicine clinical practice. However, their quality and efficacy evaluation are lacking. This study aimed to co...Objective: Granules of herbal extracts are a popular medicinal preparation consumed in traditional Chinese medicine clinical practice. However, their quality and efficacy evaluation are lacking. This study aimed to compare the quality and anti-oxidant activity of Dan Shen(Salvia miltiorrhiza Radix & Rhizoma)granule extracts with their herbal extracts.Methods: Chromatographic method was used to determine the content of 7 marker compounds in the water extracts of the herb compared to that of 12 granule extracts. Agglomerative hierarchical clustering(AHC) and principal component analysis(PCA) distinguished the herbal and granule extracts based on the content of the marker compounds. The antioxidant activities of herbal and granule extracts were evaluated by 2, 2'-azino-bis(3-ethylbenz-thiazoline-6-sulfonic acid)(ABTS), organic chemical compound 2,2-diphenyl-1-picrylhydrazyl(DPPH) and ferric ion reducing antioxidant power(FRAP) assays.Results: The herbal extracts group showed significantly higher contents of salvianolic acid B, sodium danshensu and cryptotanshinone compared with that of the granule group. This corresponded to significantly higher ABTS, DPPH and FRAP(P <.05) activities of the herbal extracts. The AHC and PCA analysis distinguished granule extracts from most herbal extracts predominantly by the content of salvianolic acid B.Conclusion: The results confirm the need for the assessment of granule products so that healthcare practitioners and consumers are better informed of their quality and efficacy.展开更多
L-Ergothioneine(L-EGT)possesses excellent antioxidant activity and has been used in the food,pharmaceuticals and cosmetics industries.In this study,a new efficient and sensitive ultra-performance liquid chromatography...L-Ergothioneine(L-EGT)possesses excellent antioxidant activity and has been used in the food,pharmaceuticals and cosmetics industries.In this study,a new efficient and sensitive ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method was established for the quantitative determination of L-EGT in food.The sample was extracted with methanol-water(70:30,V/V),separated by hydrophilic interaction liquid chromatography(HILIC)and detected by triple-quadrupole mass spectrometry.Validation studies were carried out on different product and the limit of quantitation was 20μg/kg(milk,alcohol-free beverages,dairy products)and 40µg/kg(cereal bars,chocolate).Excellent linearity(correlation coefficient(R2)≥0.999)was achieved for L-EGT quantification in the range of 5–200 ng/mL.The recoveries of the method(83.7%−107.5%)and the relative standard deviation(RSD,0.88%−6.84%(n=6))meet the performance criteria required for the determination of L-EGT in food.Finally,the applicability of the method was tested by analysing actual samples.In general,the method developed is simple,reliable,accurate,and stable and could be useful for routine analyses of L-EGT in food.展开更多
In this study,a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-codivinylbenzene),characterized,and applied as a solid-phase extraction(SPE)material.Up to 44 pharmaceuticals and personal ...In this study,a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-codivinylbenzene),characterized,and applied as a solid-phase extraction(SPE)material.Up to 44 pharmaceuticals and personal care products(PPCPs)belonging to 10 classes were recovered in environmental water samples.Different variables affecting extraction,such as adsorbent amount,sample pH,and loading speed,were optimized.Under optimal conditions,the average absolute recovgy of 44 PPCPs was 75.6%using GCHM,indicating a better performance than the commercial Oasis^HLB.SPE with home-made hydrophilic polymeric sorbent followed by ultra-performance liquid chromatography and tandem mass spectrometry was validated,and the method achieved good linearity(r2>0.991,for all analytes).In addition,the method detection limits of target compounds ranged from 0.03 to 0.6 ng/L.The developed method was applied to determine PPCPs in 10 environmental water samples taken from the Yangtze River,Huaihe River,and Taihu Lake,1 groundwater sample from Changzhou in Jiangsu Province,1 wastewater sample from Xiamen and 2 seawater samples from the Jiulong River in Fujian Province,China.In these samples,22 compounds were determined at levels ranging from 0.5 to 1590 ng/L.展开更多
基金supported by the National Science and Technology Major Project of China “Key New Drug Creation and Manufacturing Program” 2015ZX09501004-001-007National Natural Science Foundation of China 82004082Top talent training project of TCM in Henan Province。
文摘Objective: To compare the pharmacokinetic differences of the main components of Naoxintong capsule(NXTC) in normal and acute blood stasis rats. Materials and Methods: Rats were subcutaneously injected with adrenaline hydrochloride twice;during the two subcutaneous injections, the rats were placed in ice water for 4 min to reproduce the model rat of acute blood stasis. The normal and acute blood stasis rats were administrated a 5.04 g/kg dose of NXTC suspension. Then, blood samples were collected from the posterior retinal venous plexus at different time points. Plasma concentrations of four major bio-active components including caffeic acid, ferulic acid, formononetin, and tanshinone IIA in NXTC were measured using ultra-performance liquid chromatography coupled with triple-quadrupole mass spectrometry. Phoenix Win Nonlin v6.2 software was used to calculate the pharmacokinetic parameters. Results: Compared with the normal rats, the acute blood stasis rats showed a significant decrease in C_(max) of ferulic acid and formononetin, AUC_(all) of caffeic acid and ferulic acid, and AUC_(INF_obs) of ferulic acid. Conversely, an increase in the Vz_F_obs and MRT_(last) of ferulic acid and caffeic acid was observed. These findings demonstrate that the absorption of the four NXTC components was weakened in the acute blood stasis rats and that the elimination time was prolonged. Conclusions: The significant difference in some parameters of the four NXTC components between the normal and acute blood stasis rats might be caused by an increase in blood viscosity and the subsequent slowing down of blood flow in the acute blood stasis rats. The pharmacokinetic study conducted in pathological state can provide important information and scientific basis for further rational clinical application of NXTC.
基金supported by the National Key Research and Development Project(SQ2018YPC170480,2018YFC1708202)the National Natural Science Foundation of China(81774009)+1 种基金the Key science and technology projects of Inner Mongolia Autonomous Region(2019ZD004)Open Project Program of Inner Mongolia Key Laboratory of Toxicant Monitoring and Toxicology,China(MDK 2019040)。
文摘Objective:There are different geographic origins of Aconiti Kusnezoffii Radixs(AKRs)sold in the market with different quality.This study aims to establish a rapid analysis method to distinguish the different geographic origins of AKRs and to realize the rapid evaluation of their quality.Methods:An ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry(UPLC-Q-TOF MS)method was utilized to acquire the constituents'information of AKRs from different geographic origins.MSE data and Progenesis QI software were employed to identify the chemical constitutes.Principal component analysis(PCA)was applied to comparing MS data to find the chemical markers of AKRs from different geographic origins.Results:Twenty-three components were detected and 17 out of them were identified,including diester-diterpenoid alkaloids,monoester-diterpenoid alkaloids,and amine-diterpenoid alkaloids.Three pairs of isomers were detected and two of them were distinguished by the retention time of standard samples.Thirteen chemical markers were screened out through PCA and orthogonal partial least square discriminant analysis.Through detecting Napelline or isomer of Napelline(m/z 360.2530)and Aconifine(m/z 662.3170),AKRs from inner Mongolia autonomous could be screened.According to the existence of benzoylaconine(m/z 604.3108)and Indaconitine(m/z 630.3159),it could be confirmed that the AKRs are from Xinjiang Uygur autonomous.AKRs that cannot detect compounds above-mentioned could be from Liaoning or Shanxi Province.Conclusions:The chemical profile could be used not only to distinguish the AKRs from different geographic origins but also to identify the true and false of AKRs.This study lays a foundation for the study of efficacy and toxic of AKRs.
基金supported financially by the National Natural Science Foundation of China (Grant No. 81973604, 81803690and 81703684)the Innovative Talents Funding of Heilongjiang University of Chinese Medicine(Grant No.2018RCD25)+8 种基金the National natural science foundation matching project (Grant No. 2018PT02)the National natural Science Foundation Matching Project (Grant No. 2017PT01)the Graduate Innovative Research Project Foundation of Heilongjiang University of Chinese Medicine (Grant No. 2019yjscx013)the Postdoctoral Initial Fund of Heilongjiang Provincethe University Nursing Program for Young Scholars with Creative Talents in Heilongjiang Province (Grant No. UNPYSCT2017215 and UNPYSCT2017219)the Natural Science Foundation of Heilongjiang Province (Grant No. H2015037)the Heilongjiang University of Chinese Medicine Doctoral Innovation Foundation (Grant No. 2014bs05)the Application Technology Research and Development Projects of Harbin Technology Bureau (Grant No. 2014RFQXJ149)Heilongjiang Postdoctoral Scientific Research Developmental Fund (Grant No.LBHQ16210 and LBH-Q17161)
文摘A rapid and high selective ultra-performance liquid chromatography(UPLC)with tandem mass spectrometry method for simultaneous determination of six compounds including albiflorin,paeoniflorin,picroside I,picroside II,saikosaponin A,and saikosaponin D in rat plasma was developed and validated using butyl p-hydroxybenzoate as an internal standard.One-step direct protein precipitation with acetonitrile was used to extract the compounds from the rat plasma samples.Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7μm)at a flow rate of 0.4 m L/min,using gradient mode containing 0.1%formic acid in water and acetonitrile were used as the Mobile phase A and B.Electrospray ionization in negative ion mode and multiple reaction monitoring were used to identify and quantify active components.Calibration curves showed good linearity(R^2>0.9908)over a wide concentration range for all compounds.The intra-and interday precision(relative standard deviation)ranged 2.4%–7.0%and 2.6%–8.0%,respectively.The accuracy(relative error)was from-13.0%to 13.2%at all quality control levels.The recovery ranged from 81.1%to 92.5%.The validated method was successfully applied to pharmacokinetic study in rats after oral administration of Qing Gan-Shu Yu-Fang.The results show that one can draw a conclusion that these six active ingredients can be quickly absorbed and play a pharmacodynamic role rapidly in vivo.
基金supported by the Joint Chair in Traditional Chinese Medicine (JCTCM) Programfunded by the Office of Science and Research in NSW+5 种基金the University of SydneyWestern Sydney University, Australiasupported by the International Postgraduate Research Scholarship, Western Sydney Universitythe Linkage Project from the Australian Research Council (ARC) grant (LP160101594)supported by Research Support Program Fellowship, Western Sydney Universitysupported by Western Sydney University Research Grant Scheme (P00021202)。
文摘Objective: Granules of herbal extracts are a popular medicinal preparation consumed in traditional Chinese medicine clinical practice. However, their quality and efficacy evaluation are lacking. This study aimed to compare the quality and anti-oxidant activity of Dan Shen(Salvia miltiorrhiza Radix & Rhizoma)granule extracts with their herbal extracts.Methods: Chromatographic method was used to determine the content of 7 marker compounds in the water extracts of the herb compared to that of 12 granule extracts. Agglomerative hierarchical clustering(AHC) and principal component analysis(PCA) distinguished the herbal and granule extracts based on the content of the marker compounds. The antioxidant activities of herbal and granule extracts were evaluated by 2, 2'-azino-bis(3-ethylbenz-thiazoline-6-sulfonic acid)(ABTS), organic chemical compound 2,2-diphenyl-1-picrylhydrazyl(DPPH) and ferric ion reducing antioxidant power(FRAP) assays.Results: The herbal extracts group showed significantly higher contents of salvianolic acid B, sodium danshensu and cryptotanshinone compared with that of the granule group. This corresponded to significantly higher ABTS, DPPH and FRAP(P <.05) activities of the herbal extracts. The AHC and PCA analysis distinguished granule extracts from most herbal extracts predominantly by the content of salvianolic acid B.Conclusion: The results confirm the need for the assessment of granule products so that healthcare practitioners and consumers are better informed of their quality and efficacy.
基金This work was supported by National Key Research and Development Program of China(2019YFC1606400).
文摘L-Ergothioneine(L-EGT)possesses excellent antioxidant activity and has been used in the food,pharmaceuticals and cosmetics industries.In this study,a new efficient and sensitive ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method was established for the quantitative determination of L-EGT in food.The sample was extracted with methanol-water(70:30,V/V),separated by hydrophilic interaction liquid chromatography(HILIC)and detected by triple-quadrupole mass spectrometry.Validation studies were carried out on different product and the limit of quantitation was 20μg/kg(milk,alcohol-free beverages,dairy products)and 40µg/kg(cereal bars,chocolate).Excellent linearity(correlation coefficient(R2)≥0.999)was achieved for L-EGT quantification in the range of 5–200 ng/mL.The recoveries of the method(83.7%−107.5%)and the relative standard deviation(RSD,0.88%−6.84%(n=6))meet the performance criteria required for the determination of L-EGT in food.Finally,the applicability of the method was tested by analysing actual samples.In general,the method developed is simple,reliable,accurate,and stable and could be useful for routine analyses of L-EGT in food.
基金Authors gratefully acknowledge the generous support provided by the National Key R&D Program of China(Grant No.2016YFE0112300)the National Natural Science Foundation of China(Grant Nos.51678290,51438008 and 51778281)+3 种基金Jiangsu Natural Science Fund,China(No.B K 20171342)Jiangsu Provincial Key Medical Discipline(Laboratory)of China(No.Z D X K A 2016008)Jiangsu Preventive Medicine Project of China(No.Y2018081)The authors also thank Dr.Zhe Wang from Nanyang Technological University(Singapore)for his support on this project.
文摘In this study,a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-codivinylbenzene),characterized,and applied as a solid-phase extraction(SPE)material.Up to 44 pharmaceuticals and personal care products(PPCPs)belonging to 10 classes were recovered in environmental water samples.Different variables affecting extraction,such as adsorbent amount,sample pH,and loading speed,were optimized.Under optimal conditions,the average absolute recovgy of 44 PPCPs was 75.6%using GCHM,indicating a better performance than the commercial Oasis^HLB.SPE with home-made hydrophilic polymeric sorbent followed by ultra-performance liquid chromatography and tandem mass spectrometry was validated,and the method achieved good linearity(r2>0.991,for all analytes).In addition,the method detection limits of target compounds ranged from 0.03 to 0.6 ng/L.The developed method was applied to determine PPCPs in 10 environmental water samples taken from the Yangtze River,Huaihe River,and Taihu Lake,1 groundwater sample from Changzhou in Jiangsu Province,1 wastewater sample from Xiamen and 2 seawater samples from the Jiulong River in Fujian Province,China.In these samples,22 compounds were determined at levels ranging from 0.5 to 1590 ng/L.
