最新刊期
卷 43 ， 期 11 ， 2024
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摘要：This study utilized the material benchmark-based quality，combined with various research methods，to determine the optimal extraction parameters of Banxia Houpo Decoction（BHD）. Based on the concept of quality by design（QbD），key process parameters such as extraction time，water-to-material ratio，and number of decoction cycles were set，and 17 batches of freeze-dried samples of Banxia Houpo Decoction were prepared according to Box-Behnken experimental design. Taking the quality of the material-based reference sample as the standard value，through calculating the standard relation（SR） between each sample and the material-based reference，a combined method of subjective and objective weighting，namely analytic hierarchy process-entropy weight method（AHP-EWM），was used to determine the weights of five evaluation indicators：rosmarinic acid，6-gingerol，honokiol and magnolol content，yield rate and fingerprint similarity，which were determined to be 0.05，0.11，0.58，0.26，and 0，respectively. After comprehensive scoring，a predictive mathematical model was established with statistical significance. The optimal process was determined to be adding 6.32 times the amount of water，reflux extraction for 1.5 hours，and extraction for 3 times. Through repeated experiments to verify this process，the comprehensive score of BHD obtained under this process was 91.09 with a relative standard deviation（RSD） of 2.2%. The results indicate that the combination of SR-AHP-EWM method with response surface in optimizing the classical prescription extraction process for BHD ensures stability and reliability in the extraction process，with product quality attributes closely resembling those of the material-based reference. This approach has partially addressed the issue of control difficulty in transitioning from traditional to modern processes in classical prescriptions，laying a foundation for further research and industrial production of BHD while providing insights for studies on other traditional Chinese medicine formulations.关键词：Banxia Houpo Decoction;quality by design;extraction process;standard relation;analytic hierarchy process;entropy weight method;response surface method;multi-index component determination- 316
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发布时间：2024-11-26
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摘要：A high performance liquid chromatography（HPLC） method for the determination of chlorogenic acid，cryptochlorogenic acid，quercitrin，baicalin，wogonoside，baicalein and wogonin in the aqueous concentrate of Yuxingcao Qinlan Mixture was established based on the analytical quality by design（AQbD） concept. An Ishikawa diagram was employed to find all method parameters. A definitive screening design was used to clarify the critical method attributes（CMAs）. CMAs were the resolution between quercitrin and the adjacent peak，and the retention time of the last peak. The weighted determination coefficient method was utilized to find the critical method parameters（CMPs），which were the end time of the first gradient，the end time of the third gradient，the end time of the fourth gradient，column temperature and flow rate. Quantitative models between these CMPs and CMAs were then established using a stepwise regression method，with model R2 values exceeding 0.90. The non-compliance probability values were utilized to quantitatively characterize the risk level associated with different parameter combinations. Based on the risk assessment，the method operable design region（MODR） was identified and its reliability was successfully validated. The separation was achieved with a Sunshell-C18（150 mm×4.6 mm，2.6 μm） column at 39.0 ℃，using 0.60% formic acid in water（A） and acetonitrile（B） as the mobile phases in gradient elution at a flow rate of 0.80 mL/min. The elution was monitored at UV detection wavelengths of 260 nm and 326 nm. The injection volume was 10 μL.The optimized method was also validated. The results showed excellent linear regression，with the relative standard deviation（RSD） values for accuracy，precision，stability，and repeatability all less than 5.0%.All recoveries of the 7 compounds ranged from 92.6% to106%，with the RSD values of less than 2.0%.关键词：analytical quality by design;high performance liquid chromatography（HPLC）;aqueous concentrate of Yuxingcao Qinlan Mixture;definitive screening design;method operable design region- 240
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发布时间：2024-11-26 -
摘要：To establish a rapid evaluation method for seven multi-index key quality attributes of an traditional Chinese medicine Rheum tanguticum using near infrared spectroscopy（NIR），the methodologies outlined in the Chinese and Japanese pharmacopoeias were performed. The contents of seven multi-index key quality attributes of Rh. tanguticum were determined respectively，including moisture，ash，extract，bound anthraquinone，free anthraquinone，sennoside A and sennoside B. The results showed that they were in accordance with the standards of the aboved pharmacopoeia. The low water content of the samples was conducive to the storage of medicinal materials. The contents of sennoside A and sennoside B presented high level，indicating that Rh. tanguticum had a material basis for good catharsis. At the same time，membership function，principal component analysis and correlation analysis were used to comprehensively evaluate its quality. It was revealed that a great correlation between the contents of different active components was found，while ash and water content exhibited a negative correlation with certain some components. In order to further ensure the quality of this herbal medicine，it is necessary to control the range of water content and ash content. Thus，a synchronous quantitative detection model for the aforementioned eight evaluation indices，including the membership function，was established by integrating NIR with chemometrics and optimizing modeling conditions such as outlier elimination，preprocessing methods and modeling bands. In the process of model optimization，the optimal modeling conditions of each detection index were different. The evaluation metrics for water and sennoside B demonstrated the highest performance，with residual prediction deviation（RPD） values exceeding 6. The model indexes of sennoside A and membership function values were the second，and the RPD values were all greater than 3. The RPD values for extracts and free anthraquinones were above 2，while the model RPD values for total ash and total anthraquinones were comparatively lower. After external verification，the prediction rate of all indicators reached more than 85%，and the prediction rate of moisture，free anthraquinone and total anthraquinone reached more than 90%，indicating that the model had a strong prediction ability for unknown Rh. tanguticum samples. The successful establishment of the membership function value model facilitates the rapid and comprehensive quality evaluation of Rh. tanguticum. NIR combined with chemometrics methods can achieve the rapid and accurate detection of multi-index key quality attributes of Rh. tanguticum，and provide technical support for the quality evaluation and control of this medicinal material.关键词：near infrared spectrum;quality evaluation;model construction and optimization;multi-index key quality attribute;Rheum tanguticum- 275
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发布时间：2024-11-26 -
摘要：This study proposed the concept of spectral images with different dimensions，which was first applied to the identification of species in the Polygonatum genus，and established a fast and accurate identification method. A total of 563 batches of samples from 6 species of Polygonatum were collected. Five preprocessing methods were used based on Fourier transform mid infrared spectroscopy（FT-MIR），including first derivative（1st），second derivative（2nd），multiplicative scattering correction（MSC），standard normal variable（SNV） and Savitzky-Golay（SG）. Decision trees（DT），random forests（RF） and support vector machines（SVM） were constructed. In addition，to avoid complex preprocessing，a deep learning residual convolutional neural network（ResNet） model was constructed to draw spectral images of different dimensions，including 10 datasets of one-dimensional MIR，synchronous，asynchronous，and integrative two-dimensional correlated spectra，three-dimensional correlated spectra，and three-dimensional correlated spectral projection images，and they were combined with the ResNet model for classification. The results showed that different preprocessing methods have different impacts on the model results，and the MSC preprocessing method significantly improved the accuracy of the DT，RF，and SVM algorithms. The ResNet algorithm based on synchronous two-dimensional correlated spectral dataset had the best modeling effect，with an accuracy of 100%，small loss value，no need for complex preprocessing，low time cost，and could accurately identify species of Polygonatum genus，providing reference for identification in other fields such as food and traditional Chinese medicine.关键词：species of Polygonatum genus;Fourier transform mid infrared spectroscopy;spectral images of different dimensions;machine learning algorithms;residual neural networks- 214
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发布时间：2024-11-26 -
摘要：By comparing the model performance of random forest（RF），support vector machine（SVM），principal component analysis support vector machine（PCA-SVM），and convolutional neural network（CNN），the optimal model for rapid microbial limit prediction based on surface enhanced Raman spectroscopy（SERS） technology was obtained，providing a new method for rapid microbial limit prediction of intermediates in traditional chinese medicine（TCM） formulations. First，Au@Ag@SiO2 composite nanomaterials were synthesized as SERS reinforcement substrates. Secondly，a double-layer membrane filtration method was used to prepare the intermediate test sample of TCM preparations，and the antibacterial activity of the sample was investigated. Finally，SERS spectra of 30 batches of intermediate samples from TCM preparations were collected，and RF，SVM，PCA-SVM，and CNN fast prediction models based on ResNet architecture were established，respectively. The results showed that the accuracy，precision，and recall of the established CNN model were all 100.0%，with an F1 score of 1.0. The receiver operating characteristic（ROC） curve showed that the CNN model had higher rapid prediction ability for the total aerobic bacterial count（TAMC），total mold and yeast count（TYMC） of TCM intermediates than the other three algorithms. It can effectively predict the microbial limit of the test sample，provide effective risk warning for unqualified samples，and improve the quality control level of intermediate microorganisms in the production process of TCM.关键词：surface enhanced Raman scattering（SERS）;machine learning;microbial limit testing;rapid prediction- 267
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发布时间：2024-11-26 -
摘要：In this work，a high performance liquid chromatography-diode array detector（HPLC-DAD） was used to establish a quantitative method for the determination of six organic acids in Ginkgo biloba extract based on analytical quality by design（AQbD） concept. Firstly，potential critical method parameters（CMPs） were identified by Ishikawa diagram. Then the critical method attributes（CMAs） were identified by definitive screening design. A stepwise regression method was used to build quantitative models between CMAs and CMPs. The method operable design region was established by a probability-based method and verified successfully. The analytical method robustness was tested using the Plackett-Burman design. The method was verified and can be used for the determination of organic acids in Ginkgo biloba extract.关键词：Ginkgo biloba;analytical quality by design;design of experiment;method operable design region;organic acids;high performance liquid chromatography- 168
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发布时间：2024-11-26 -
摘要：The identification of different sources of licorice is of great significance for ensuring its clinical application. Based on the spectral features of 89 licorice medicinal materials from three sources，including Glycyrrhiza uralensis Fisch.，Glycyrrhiza inflata Bat.，and Glycyrrhiza glabra L.，11 texture feature parameters（short run emphasis，long run emphasis，gray-level non-uniformity，run-length non-uniformity，run percentage，low gray-level run emphasis，high gray-level run emphasis，short run low gray-level emphasis，short run high gray-level emphasis，long run low gray-level emphasis，long run high gray-level emphasis） were extracted using the gray-level run-length matrix from four perspectives（0°，45°，90°，and 135°）. Through an innovative feature selection method-normalized average discrepancy method，texture features with significant contributions were selected and fused with spectral features to improve the accuracy of source identification. Compared to traditional feature selection methods such as SelectKBest（SKB），recursive feature elimination（RFE），and SelectFromModel（SFM），the normalized average discrepancy method demonstrated higher applicability in the dataset of this study，with a source identification accuracy of 95.28% on the test set using support vector machine（SVM） classifier，higher than the unselected（92.22%），SKB-selected（95.00%），RFE-selected（95.00%），and SFM-selected（93.89%） accuracies. The data mining method proposed in this study fully utilizes the hyperspectral data and image data，integrating spectral features and texture features，providing a new non-destructive analytical techniques for the source identification of licorice medicinal materials.关键词：licorice;source identification;hyperspectral imaging technology;machine learning;gray-level run-length matrix;feature selection- 237
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发布时间：2024-11-26 -
摘要：A quantitative method and a fingerprint method were established for a total of 10 components in Xiaochaihu Capsules，including liquiritin，lobetyolin，baicalin，wogonoside，baicalein，licoricesaponin G2，glycyrrhizin，wogonin，saikosaponin B2 and saikosaponin B1. They were analyzed by ultra high performance liquid chromatography（UHPLC）. Waters HSS T3 chromatographic column（100 mm×2.1 mm，1.8 μm） was used. The mobile phase was consisted of 0.05% phosphoric acid solution and acetonitrile. The elution mode was gradient elution. The detection wavelength was set at 215 nm and 254 nm by diode-array detector（DAD）. There were 22 common peaks in the fingerprints. The ultra high performance liquid chromatography quadrupole time of flight mass spectrometry（UHPLC-Q-TOF MS） was used to infer the structure of the compounds in the common peaks. The relative standard deviations（RSDs） of precision，repeatability and stability were all less than 6.0%. The linear relationship of 10 components was good within the quantitative range. The determination coefficients（r2） were higher than 0.999. RSDs of injection precision and method repeatability were less than 6.0%. The sample solution was stable within 24 hours，and the recoveries of each component were 91.9%-104%. 12 batches of Xiaochaihu Capsules from different batches were analyzed using the established analytical method. The results showed good consistence of Xiaochaihu Capsules among different batches. The established analytical method is stable，accurate and reliable. It can be used to detect the index components in Xiaochaihu Capsules. The detection results can reflect the quality of Xiaochaihu Capsules more comprehensively.关键词：Xiaochaihu Capsules;fingerprint;content determination;UHPLC;dual-wavelength detection- 115
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发布时间：2024-11-26 -
摘要：A quantitative content determination method was established for four intermediates for the extraction of concentrate，thick paste，extract powder and granulation powder from Xiaochaihu Capsules. The quantitative content were including liquiritin，lobetyolin，baicalin，wogonoside，baicalein，licoricesaponin G2，glycyrrhizin，wogonin，saikosaponin B2 and saikosaponin B1. The detected substances were analyzed by ultra-high performance liquid chromatography（UHPLC）. HSS T3 chromatographic column（100 mm×2.1 mm，1.8 μm） was used. The mobile phase was consisted of 0.05% phosphoric acid solution and acetonitrile. The elution mode was gradient elution. The detection wavelength was set at 215 nm and 254 nm. The linear relationship of 10 quantitative components was good within the certain mass concentration ranges and the correlation coefficients（r2） were all more than 0.999. Relative standard deviations（RSDs） of injection precision and method repeatability met the requirements of the pharmacopoeia. The sample solution was stable within 24 hours，and the recoveries of each component met the requirements of the pharmacopoeia. The method was used to determine the attribution of 23 chromatographic peaks after comparing with the obtained by lack of herb intermediates. 4 intermediates in 8 batches were used to analyze Xiaochaihu Capsule intermediates by the established method. The established analytical method is stable，accurate and reliable. It provides technical support for the improvement of the pharmaceutical process of Xiaochaihu Capsules.关键词：Xiaochaihu Capsules;intermediates;content determination;concentrate;UHPLC- 187
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发布时间：2024-11-26 -
摘要：This study aims to establish benchmark samples of Banxia Houpo Decoction（BHD） using ultra performance liquid chromatography（UPLC） fingerprinting and a multi-component quantitative analysis method，and to thoroughly investigate the quantitative transmitting，laying the foundation for further research on BHD compound preparations. Based on the previous literature review to confirm the formulation composition，15 batches of BHD reference samples were prepared，and a UPLC fingerprint was established，with peak assignment and similarity analysis conducted. Subsequently，methods for determining the content of rosmarinic acid，6-gingerol，honokiol and magnolol in BHD were developed. By measuring the content of multiple components in the material standard，a study on the transfer laws from crude herbs to substance benchmark was carried out. The study revealed that the BHD benchmark samples fingerprint displayed 16 common peaks，with a similarity to the control fingerprint exceeding 0.95. Identified chromatographic peaks included caffeic acid，scutellarin，rosmarinic acid，6-gingerol，honokiol，and magnolol. The average transfer rates of each indicator component from crude herbs to material standard were as follows：rosmarinic acid at 81.77%，with a transfer rate range of 64.57% to 110.96%；6-gingerol at 28.58%，with a transfer rate range of 11.22% to 36.94%；honokiol and magnolol at 3.51%，with a transfer rate range of 1.60% to 6.03%. By combining the fingerprinting and multi-indicator component content determination model，the quantitative transmitting law of BHD benchmark samples was summarized，and a stable and reliable quality evaluation method of BHD benchmark samples was initially established，which provides a certain reference for the quality control of the classical prescription preparation and the subsequent research on the preparation of BHD.关键词：Banxia Houpo Decoction;benchmark samples;quantitative transmitting;fingerprint;content determination- 250
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发布时间：2024-11-26 -
摘要：Ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry （UPLC-Q-TOF-MS/MS） combined with multivariate statistical method was used to analyze the quality differences of Microctis Folium from different producing areas，so as to provide basis for the origin discrimination and quality evaluation of Microctis Folium. UPLC-Q-TOF-MS/MS was used to analyze the total components of Microctis Folium samples from different producing areas. The principal component analysis（PCA），orthogonal partial least squares discriminant analysis（OPLS-DA） and cluster analysis（CA） were used to analyze 18 batches of Microctis Folium from Kunming of Yunnan Province，Yulin of Guangxi Province and Yangjiang of Guangdong Province. According to VIP > 1 and t test（P<0.05），the chemical components with significant differences in Microctis Folium from different producing areas were screened. A total of 53 chemical components were identified from Microctis Folium of different habitats，which were mainly flavonoids，procyanidins，organic acids and alkaloids. Among them，N-p-trans-coumaroyltyramine and N-trans-feruloyltyramine were reported in Microctis Folium for the first time. The chemical components of Microctis Folium from different producing areas were significantly different，and a total of 17 differential chemical components were identified. 17 differential chemical components showed different variation rules in different producing areas，which can be used as the basis for the identification of producing areas.关键词：Microctis Folium;UPLC-Q-TOF-MS/MS;multivariate statistical analysis;differences of production area;quality evaluation- 234
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发布时间：2024-11-26 -
摘要：The experiment combined multiple research methods to determine the optimal extraction process for the classical formula Qingjin Huatan Decoction. Based on the concept of quality by design（QbD），critical quality attributes（CQAs），including the water addition ratio，extraction time，and extraction frequency were selected. Seventeen sets of freeze-dried samples of QJHTD were prepared according to the Box-Behnken Design（BBD）. Calculated the standard relationship（SR） between each group of samples and the material-based reference sample，using the quality of the material-based sample as the reference value. The analytic hierarchy process（AHP）-entropy weight method（EWM） method，which combined subjective and objective methods，the weight coefficients of geniposide，mangiferin，baicalin，glycyrrhizic acid，yield rate，and fingerprint similarity were determined to be 0.529，0.127，0.083，0.055，0.206，and 0.000，respectively. After comprehensive evaluation，the established mathematical model has statistical significance. The optimal extraction process parameters for QJHTD were determined to be adding 6 times the amount of water，extracting for 30 minutes，and extracting once. The repeated test results showed that the average comprehensive score was 90.865，which meet the requirements of the quality control standard for the material-based reference sample of QJHTD. This indicated that the optimized process parameters were more stable and reliable，laid a foundation for the subsequent preparation of QJHTD granules. In addition，the comprehensive experimental design method combining response surface methodology with SR-AHP-EWM can provide ideas for future research on other classic formulas.关键词：Qingjin Huatan Decoction;standard relation;extraction process;analytic hierarchy process and entropy weight method（AHP-EWM）- 285
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发布时间：2024-11-26 -
摘要：Based on ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry（UPLC-Q-TOF-MS/MS） and ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry（UPLC-QQQ-MS/MS），a method for the analysis of the chemical components of chamomile was established in this research. UPLC-Q-TOF-MS/MS was performed on a Waters ACQUITY UPLC BEH C18 column（150 mm×2.1 mm，1.7 μm），and UPLC-QQQ-MS/MS was performed on an Agilent Extend-C18 column（100 mm×2.1 mm，1.8 μm） using a gradient elution of methanol -0.1% formic acid aqueous as the mobile phase，and then analyzed in both electrospray ionization and negative ion modes. A total of 34 chemical components was identified，include of flavonoids and organic acids，among which onsalin，myricetin 3-O-β-D-pyranogalactoside and isrhamhamin-O-hexoside were the first reported components of chamomile. In addition，five chlorogenic acid components were quantitatively analyzed in chamomile by UPLC-QQQ-MS/MS. The relative standard deviations（RSDs） of precision，stability and reproducibility of the index components were no more than 4.0%，and the linearity of the five components was good（r≥0.999 2） with the average spiked recoveries of 99.8%-104%. This method is accurate and efficient，and can provide experimental basis and theoretical foundation for chamomile quality standard and medicinal substances.关键词：UPLC-Q-TOF-MS/MS;UPLC-QQQ-MS/MS;chamomile;chemical components;qualitative analysis;quantitative analysis- 184
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发布时间：2024-11-26 -
摘要：To establish a quantitative analytical model based on near infrared spectroscopy（NIRS） technique to rapidly predict the content of polysaccharides，total saponins and total phenols in Polygonatum kingianum Coll. et Hemsl. The contents of the three active ingredients of 116 batches of P. kingianum samples were determined by UV-Vis spectrophotometry. At the same time，the near infrared spectra of the samples were collected by NIRS technique，and after the anomalous spectra were eliminated，the optimal spectral model was selected by combining the multiplicative scattering correction（MSC），the first derivative（1stD），the second derivative（2ndD） and S-G smoothing（S-G）etc. were used to screen the optimal spectral preprocessing，and the partial least squares（PLS） method was used to establish the quantitative models of polysaccharides，total saponins and total phenols in P. kingianum，and the optimal quantitative models were screened by external validation. The best quantitative models were developed by choosing MSC+2ndD+S-G，MSC+1stD+NS，MSC+1stD+S-G pretreatment methods for polysaccharides，total saponins and total phenols，respectively，with the wavenumbers of 8 000-4 000 cm-1 and the numbers of principal components of 6，13 and 13. The correlation coefficients of training set（Rcal） is 0.923，0.990 and 0.938，respectively，and the correlation coefficients of verification set（Rpre） is 0.924，0.901 and 0.910，respectively，which showed good correlation. The root mean square error of prediction（RMSEP） is 5.380%，0.478%，and 0.028 mg·g-1，and the ratio of performance to deviation（RPD） is 2.11，2.16 and 1.95，respectively. The average relative deviations were less than 2.0%. The established quantitative model of P. kingianum is accurate and reliable，which proves that the NIRS technique is a feasible，accurate and rapid nondestructive testing method for the rapid determination of the active ingredients in P. kingianum.关键词：Polygonatum kingianum Coll. et Hemsl;polysaccharide;total saponins;total phenols;near infrared spectroscopy;quantitative analysis model- 214
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发布时间：2024-11-26
Scientific Papers
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摘要：To establish a multivariate statistical process control（MSPC） model for the extraction process of Xuefu Zhuyu capsules，and to monitor the extraction process on-line. Near infrared（NIR） spectrometer was used to collect spectral data of on-line extraction process of multiple batches of Xuefu Zhuyu capsules. The process spectra were used for principal component analysis（PCA） to establish a trajectory chart of the extraction process of Xuefu Zhuyu capsules，it reflects the trend of the extraction process over time. In addition，a principal component score（PC score），DModX，and Hotelling T2 control models were established in conjunction with MSPC to monitor the extraction process. The PC score charts，DModX charst，and Hotelling T2 control charts were generated. The PC1 score chart uses ±3 SD as the control limit，reflecting the fluctuation of PC with the process state；The DModX control chart uses +3 SD as the control limit，reflecting the absolute distance of sampling points from the model，and is a measure of the degree of external data changes in the model；The Hotelling T2 chart uses 95% as the control limit，reflecting the distance of sampling points from the center of the PCA model for each batch. Establishing three MSPC control models using process spectra from normal batches can directly observe the overall changes in the extraction process of Xuefu Zhuyu capsules. The combination of the three control models can timely and accurately identify batches with abnormal water addition，extraction temperature，and missing materials. MSPC technology is faster and more non-destructive compared with traditional off-line detection methods.The combination of NIRS and MSPC technology can be fully applied to on-line monitoring of the extraction process of Xuefu Zhuyu capsules，which has reference significance for improving the quality of traditional Chinese medicine production.关键词：near infrared spectroscopy;multivariate statistical process control;Xuefu Zhuyu capsules;on-line monitoring;principal component analysis- 208
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发布时间：2024-11-26 -
摘要：An ultra-high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） was developed for the determination of ethephon residue in traditional Chinese medicine. The traditional Chinese medicine samples were extracted and frozen with 50% methanol solution containing 1% formic acid after crushing，diluted with acetonitrile，purified by octadecyl bonded Silica gel（C18），silica gel，graphitized carbon black（GCB），with 1.2% formic acid aqueous solution and 0.5% formic acid acetonitrile as mobile phase. Anionic Polar Pesticide Column（2.1 mm×100 mm，5 μm） was used to separate the pesticide in 15 min. Multiple reaction monitoring（MRM） mode was used in electrospray negative ion mode，and structural similarity was used as internal standard. The results showed that ethephon in 9 kinds of traditional Chinese medicine were linear（r＞0.99） in the corresponding mass concentration ranges，and the limits of detection（LODs） and limits of quantitation（LOQs） were 0.5-1.0 μg/kg and 10-20 μg/kg，respectively. The average recoveries with three concentration levels were 71.6%-91.5%，77.1%-97.6% and 84.7%-99.5%，with the intra-day relative standard deviations（RSDs） less than 6.5%. The method was applied to 93 batches of actual samples，and the detection rate of ethephon was 68.8%. The method is time-saving，convenient and sensitive，and can meet the requirements of detecting ethephon residue in most traditional Chinese medicine.关键词：UPLC-MS/MS;ethephon;traditional Chinese medicine;residue detection- 170
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发布时间：2024-11-26 -
摘要：The analysis was achieved by high-performance liquid chromatography（HPLC） and similarity of fingerprints evaluation. Additionally，principal component analysis（PCA） and orthogonal partial least squares discriminate analysis（OPLS-DA） were employed to explorate the overall data and differential compounds of Fufang Nanbanlangen Keli. At the same time，taking aesculetin as the internal standard，relative correction factors of caftaric acid and chicoric acid were calculated to establish the multi-components by single marker（QAMS） method. The correctness and practicability of this study was assessed by contrasting the data with external standard method（ESM）. 13 common chromatographic peaks were signed in fingerprints with 10 batches of Fufang Nanbanlangen Keli，and the similarities of each batch were 0.942-0.996. The PCA and OPLS-DA study showed that there were certain varies from different manufacturers. Compared with ESM data，the data of QAMS method were not significantly different. The established fingerprint combined with QAMS method are econimic and reliable，which can provide references and systematic studies for the comprehensive supervisory control of Fufang Nanbanlangen Keli.关键词：Fufang Nanbanlangen Keli;characteristic fingerprint;QAMS;aesculetin;high-performance liquid chromatography- 252
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发布时间：2024-11-26 -
摘要：The volatile components of Polygonatum sibiricum from Mount Tai were identified by gas chromatography-ion mobility spectrometry （GC-IMS），and 60 batches Polygonatum sibiricum from Mount Tai and Qinling Mountains were distinguished by GC-IMS combined with multivariate statistical analysis. The volatile components visible fingerprint of the samples were generated by LAV plug-in of the instrument，and qualitative analysis was carried out by the built-in NIST gas chromatography retention index database and IMS migration time database. The principal component analysis （PCA） and orthogonal partial least squares analysis（OPLS-DA） were employed to distinguish Polygonatum sibiricum samples from different regions，and VIP and t-test were used to screen the differential components. A total of 72 volatile components were identified from Polygonatum sibiricum，including 19 aldehydes，13 esters，12 ketones，13 alcohols，9 terpenoids and 6 others. Among the identified volatile components，the number of aldehydes is large，accounting for 26.4% of the known substances detected. PCA analysis showed that Polygonatum sibiricum from Mount Tai could be well clustered together，which indicated that the volatile components in Polygonatum sibiricum samples from this area were similar. The Polygonatum sibiricum samples from Mountain Tai and Qinling Mountains could be well classified via combining GC-IMS and OPLS-DA method，and 20 differential components （VIP>1.2，P<0. 05） were screened out，mainly aldehydes and ketones. The contents of 2-methylbutyric acid，2-methyl-1-propanol，hydroxyacetone，2-methyltetrahydrofuran-3-one and 3-hydroxy-2-butanone are higher in Polygonatum sibiricum from the Mount Tai. The results of clustering heat map analysis verified that these 20 components in Polygonatum sibiricum from different regions could reflect the characteristics of Polygonatum sibiricum from Mount Tai and Qinling Mountains，which are expected to be used as markers for the identification of Polygonatum sibiricum from Mount Tai. At the same time，the experimental results show that GC-IMS technology has the characteristics of simple sample pretreatment and strong visualization，and it can more intuitively represent the composition and content difference of volatile components. This study provided method and data support for the authenticity evaluation and quality control of Polygonatum sibiricum from Mount Tai.关键词：gas chromatography-ion mobility spectrometry;Polygonatum sibiricum;volatile components;origin distinction;multivariate statistical analysis- 170
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发布时间：2024-11-26 -
摘要：A qualitative and quantitative method for the quality evaluation of Polygoni Onrientalis Fructus was established，which is based on the the reference traditional Chinese medicinal materials and quantitative without relying on multiple reference substances. The chromatogram of Polygoni Onrientalis Fructus was established by using high performance liquid chromatography （HPLC） technology and dual wavelength differential fusion technology. The authenticity of the medicinal materials was confirmed by the calibration of characteristic peaks. The internal standard component texifolin was accurately quantified，the relative content of each characteristic peak was calculated based on texifolin，and "mean-standard deviation" was taken as the lower limit of the relative content of the characteristic peak component relative to the chemical composition of the internal standard substance. As a result 10 common characteristic peaks of Polygoni Onrientalis Fructus were identified，and 7 components were identified by mass spectroscopy（MS）. By comparing the reference products，three chemical components of the common characteristic peaks were identified，namely，texifolin，quercetin and protocatechuic acid. The content of texifolin in each batch of medicinal materials was 0.599 4%-0.776 6%. The lower limit of relative content of chemical components of Polygoni Onrientalis Fructus characteristic peak was defined.The method can judge the authenticity of the herbs clearly without relying on many reference products，and provide reference for the quality control method of Polygoni Onrientalis Fructus.关键词：Polygoni Onrientalis Fructus;Control medicinal materials;quality control;Characteristic Spectrum;Dual wavelength differential fusion;high performance liquid chromatography- 204
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发布时间：2024-11-26 -
摘要：The feasibility of UV-visible（UV-Vis） diffuse reflectance spectroscopy combined with chemometrics for the identification of Angelicae Sinensis Radix（ASR） and its adulterants was investigated in this research. A total of 40 pure and 75 adulterated ASR samples were prepared. The Kennard-Stone（KS） grouping method was firstly used to divide the dataset into a training set with 86 samples and a prediction set with 29 samples. Then the raw spectra and the preprocessed spectra by continuous wavelet transform（CWT），CWT-SG smoothing，and CWT- SG smoothing-autoscaling are analyzed. Spectra and their corresponding principal component analysis（PCA） plots were used to determine the optimal preprocessed method. Finally，partial least squares-discriminant analysis（PLS-DA） was used to build discrimination model. The results showed that PCA of the raw UV-Vis spectra could not separate ASR from their adulterated products. After the spectra preprocessed by CWT-SG smoothing-autoscaling，not only the pure ASR and its adulterants can be completely separated in the principal component space，but also the adulterants with different contents can be further identified. The optimal preprocessing method combined with PLS-DA can achieve 100% prediction accuracy for the identification of ASR with its adulterants in prediction set with one factor. Therefore，UV-Vis combined with CWT-SG smoothing-autoscaling PLS-DA is a rapid and accurate method for discriminating ASR and its adulterants.关键词：Angelicae Sinensis Radix;adulterants;visual identification;ultraviolet-visible diffuse reflectance spectroscopy;principal component analysis;chemical pattern recognition;preprocessing- 224
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发布时间：2024-11-26
Experimental Techniques and Methods
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