A simple, sensitive and accurate method based on high performance liquid chromato- graphy (HPLC) with diode array detector (DAD) was developed and validated for systematic quality evaluation of one type of traditi...A simple, sensitive and accurate method based on high performance liquid chromato- graphy (HPLC) with diode array detector (DAD) was developed and validated for systematic quality evaluation of one type of traditional Chinese medicine preparations named Xinkeshu (XKS) tablet. In this study, the chromatographic fingerprints of XKS tablet were developed first, 23 peaks were selected as the common peaks to evaluate the similarities among different batches of XKS samples, which were manufactured in a long time span of three years. Additionally, simultaneous quantification of six markers in XKS tablet, including Danshensu, Protocatechuic aldehyde, Puerarin, Daidzin, Salvianolic acid B and Daidzein, was performed. The validation results showed that the developed method was specific, accurate, precise and robust. The preliminary explanation on why a close similarity between fingerprints did not exactly mean similar contents of chemical components in samples was given. The contribution of each chromatographic peak to similarity was also evaluated. The developed method offers an efficient, reliable and practical approach for systematic quality evaluation of XKS tablet.展开更多
Near infrared(NIR)spectroscopy has been developed into one of the most important process analytical techniques(PAT)in a wide field of applications.The feasibility of NIR spectroscopy with partial least square regressi...Near infrared(NIR)spectroscopy has been developed into one of the most important process analytical techniques(PAT)in a wide field of applications.The feasibility of NIR spectroscopy with partial least square regression(PLSR)to monitor the concentration of paeoniflorin,albi-florin,gallic acid,and benzoyl paeoniforin during the water extraction process of Radix Paeoniae Alba was demonstrated and verified in this work.NIR spectra were collected in transmission mode and pretreated with smoothing and/or derivative,and then quantitative models were built up using PLSR.Interval partial least squares(iPLS)method was used for the selection of spectral variables.Determination coeficients(R2aI and R2red),root mean squares error of prediction(RMSEP),root mean squares error of calibration(RMSEC),and residual predictive deviation(RPD)were applied to verify the performance of the models,and the corresponding values were 0.9873 and 0.9855,0.0487 mg/mL,0.0545mg/mL and 8.4 for paeoniforin;0.9879,0.9888,0.0303 mg/mL,0.0321 mg/mL and 9.1 for albiflorin;0.9696,0.9644,0.0140 mg/mL,0.0145 mg/mL and 5.1 for gallic acid;0.9794,0.9781,0.00169 mg/mL,0.00171 mg/mL and 6.9 for benzoyl paeoniflorin,respectively.The results turned out that this approach was very efficient and environmentally friendly for the quantitative monitoring of the water extraction process of Radix Paeoniae Alba.展开更多
Objective Due to the complicated compounds and the synergistic effect of multi-compounds,the quality control and assessment of Chinese materia medica(CMM)encounters a great challenge about how to identify the key comp...Objective Due to the complicated compounds and the synergistic effect of multi-compounds,the quality control and assessment of Chinese materia medica(CMM)encounters a great challenge about how to identify the key compounds,which are directly correlated with its efficacy and safety.On the guidance of study on quality marker(Q-Marker),identification of Q-Markers was performed from Hedan Tablet(HDT)by the aid of the“spider-web”mode and hepatotoxicity evaluation derived from our previous researches and literatures.Methods By the established ultra performance liquid chromatography with photodiode array detector(UPLC-PDA)method,online UPLC-DPPH·and offline antioxidant assay,21 candidate compounds of HDT were systematically investigated and comprehensively evaluated by the“spider-web”mode for them properties of Q-Marker based on“content-stability-activity”.In addition,the Q-Markers related with hepatotoxicity based on our previous researches and literatures were identified.Results Salvianolic acid B(SaB),quercetin-3-O-glucuronide(Qug),isoquercitrin(IQ)and hyperoside(Hyp)were adopted as the preferable Q-Markers of HDT according to the shaded area(A)of tested compounds in“spider-web”mode.Psoralen(Ps),isopsoralen(IP),psoralenoside(PO)and isopsoralenoside(IPO)were also strongly recommended as Q-Markers closely related with safety by considering hepatotoxicity of the accumulated Ps and IP and conversion between glycoside(PO and IPO)and aglycone(Ps and IP).Conclusion This study provided scientific evidence for quality control and assessment of HDT,and also provided a meaningful reference for application of Q-Markers in CMM.展开更多
基金supported by the Major Projects of Independent Innovation Achievements of Shandong Province(No. 2010ZDZX1A0406)partly by the Scientific and Technological Projects of Shandong Province (No. 2009GG10002081)+1 种基金Independent Innovation Foundation of Shandong University(No. 2010TS054)Shandong Province Natural Science Foundation, China (No. ZR2011HM080)
文摘A simple, sensitive and accurate method based on high performance liquid chromato- graphy (HPLC) with diode array detector (DAD) was developed and validated for systematic quality evaluation of one type of traditional Chinese medicine preparations named Xinkeshu (XKS) tablet. In this study, the chromatographic fingerprints of XKS tablet were developed first, 23 peaks were selected as the common peaks to evaluate the similarities among different batches of XKS samples, which were manufactured in a long time span of three years. Additionally, simultaneous quantification of six markers in XKS tablet, including Danshensu, Protocatechuic aldehyde, Puerarin, Daidzin, Salvianolic acid B and Daidzein, was performed. The validation results showed that the developed method was specific, accurate, precise and robust. The preliminary explanation on why a close similarity between fingerprints did not exactly mean similar contents of chemical components in samples was given. The contribution of each chromatographic peak to similarity was also evaluated. The developed method offers an efficient, reliable and practical approach for systematic quality evaluation of XKS tablet.
基金the financial support of the Basal Research Fund Project of Shandong University(No.2015YQ010).
文摘Near infrared(NIR)spectroscopy has been developed into one of the most important process analytical techniques(PAT)in a wide field of applications.The feasibility of NIR spectroscopy with partial least square regression(PLSR)to monitor the concentration of paeoniflorin,albi-florin,gallic acid,and benzoyl paeoniforin during the water extraction process of Radix Paeoniae Alba was demonstrated and verified in this work.NIR spectra were collected in transmission mode and pretreated with smoothing and/or derivative,and then quantitative models were built up using PLSR.Interval partial least squares(iPLS)method was used for the selection of spectral variables.Determination coeficients(R2aI and R2red),root mean squares error of prediction(RMSEP),root mean squares error of calibration(RMSEC),and residual predictive deviation(RPD)were applied to verify the performance of the models,and the corresponding values were 0.9873 and 0.9855,0.0487 mg/mL,0.0545mg/mL and 8.4 for paeoniforin;0.9879,0.9888,0.0303 mg/mL,0.0321 mg/mL and 9.1 for albiflorin;0.9696,0.9644,0.0140 mg/mL,0.0145 mg/mL and 5.1 for gallic acid;0.9794,0.9781,0.00169 mg/mL,0.00171 mg/mL and 6.9 for benzoyl paeoniflorin,respectively.The results turned out that this approach was very efficient and environmentally friendly for the quantitative monitoring of the water extraction process of Radix Paeoniae Alba.
基金supported by Science and Technology Program of Tianjin(20ZYJDJC00070)National Key R&D Program of China(2018YFC1704500)TCM Standardization Project Supported by State Administration of Traditional Chinese Medicine(ZYBZHC-JX-38)。
文摘Objective Due to the complicated compounds and the synergistic effect of multi-compounds,the quality control and assessment of Chinese materia medica(CMM)encounters a great challenge about how to identify the key compounds,which are directly correlated with its efficacy and safety.On the guidance of study on quality marker(Q-Marker),identification of Q-Markers was performed from Hedan Tablet(HDT)by the aid of the“spider-web”mode and hepatotoxicity evaluation derived from our previous researches and literatures.Methods By the established ultra performance liquid chromatography with photodiode array detector(UPLC-PDA)method,online UPLC-DPPH·and offline antioxidant assay,21 candidate compounds of HDT were systematically investigated and comprehensively evaluated by the“spider-web”mode for them properties of Q-Marker based on“content-stability-activity”.In addition,the Q-Markers related with hepatotoxicity based on our previous researches and literatures were identified.Results Salvianolic acid B(SaB),quercetin-3-O-glucuronide(Qug),isoquercitrin(IQ)and hyperoside(Hyp)were adopted as the preferable Q-Markers of HDT according to the shaded area(A)of tested compounds in“spider-web”mode.Psoralen(Ps),isopsoralen(IP),psoralenoside(PO)and isopsoralenoside(IPO)were also strongly recommended as Q-Markers closely related with safety by considering hepatotoxicity of the accumulated Ps and IP and conversion between glycoside(PO and IPO)and aglycone(Ps and IP).Conclusion This study provided scientific evidence for quality control and assessment of HDT,and also provided a meaningful reference for application of Q-Markers in CMM.