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ObjectiveTo screen the differential markers by analyzing volatile components in Dalbergia odorifera and its counterfeits， in order to provide reference for authentication of D. odorifera. MethodThe volatile components in D. odorifera and its counterfeits were detected by headspace gas chromatography-mass spectrometry（HS-GC-MS）， and the GC conditions were heated by procedure（the initial temperature of the column was 50 ℃， the retention time was 1 min， and then the temperature was raised to 300 ℃ at 10 ℃ for 10 min）， the carrier gas was helium， and the flow rate was 1.0 mL·min-1， the split ratio was 10∶1， and the injection volume was 1 mL. The MS conditions used electron bombardment ionization（EI） with the scanning range of m/z 35-550. The compound species were identified by database matching， the relative content of each component was calculated by the peak area normalization method， and principal component analysis（PCA）， orthogonal partial least squares-discrimination analysis（OPLS-DA） and cluster analysis were performed on the detection results by SIMCA 14.1 software， and the differential components of D. odorifera and its counterfeits were screened out according to the variable importance in the projection（VIP） value>2 and P<0.05. ResultA total of 26， 17， 8， 22， 24 and 7 volatile components were identified from D. odorifera， D. bariensis， D. latifolia， D. benthamii， D. pinnata and D. cochinchinensis， respectively. Among them， there were 11 unique volatile components of D. odorifera， 6 unique volatile components of D. bariensis， 3 unique volatile components of D. latifolia， 6 unique volatile components of D. benthamii， 8 unique volatile components of D. pinnata， 4 unique volatile components of D. cochinchinensis. The PCA results showed that， except for D. latifolia and D. cochinchinensis， which could not be clearly distinguished， D. odorifera and other counterfeits could be distributed in a certain area， respectively. The OPLS-DA results showed that D. odorifera and its five counterfeits were clustered into one group each， indicating significant differences in volatile components between D. odorifera and its counterfeits. Finally， a total of 31 differential markers of volatile components between D. odoriferae and its counterfeits were screened. ConclusionHS-GC-MS combined with SIMCA 14.1 software can systematically elucidate the volatile differential components between D. odorifera and its counterfeits， which is suitable for rapid identification of them.
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The study aimed to evaluate the composition and diversity of algae in the JP Lake of Jahangirnagar University campus. The research was carried out between the period of December 2021 to November 2022. A total of 72 water samples were used to carry out the investigation. Shannon and Simpson diversity indexes were used to determine the level of diversity. 234 phytoplankton species under 98 genera were found belonging to 8 classes (Cyanophyceae, Chlorophyceae, Bacillariophyceae, Synurophyceae, Euglenophyceae, Cryptophyceae, Dinophyceae, and Xanthophyceae). According to the generic percentage composition, Chlorophyceae comprised 46%, followed by Bacillariophyceae (20%) and Cyanophyceae (18%). At the species level, Euglenophyceae were found to dominate (34%) the studied sites that were followed by Chlorophyceae (31%) and Cyanophyceae (18%). The total density of phytoplankton was 387.34×105 ind/l. The highest phytoplankton density was found in April, and the lowest one was in November. Cell dispersion was below average in May for Cyanophyceae, Bacillariophyceae, Cryptophyceae, and Synurophyceae. Oscillatoria, Monoraphidium, Actinastrum, Cosmarium, Trachelomonas, and Euglena dominated the surveyed region. The Shannon Diversity Index showed a value of 1.51, while Simpson's Diversity Index showed a value of 0.28. The overall variation (80.73%) among the classes was represented by PCA cells. According to the Shannon and Simpson Diversity Indexes, the diversity was low.
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ObjectiveTo compare the effects of different processing methods in ancient and modern times on the chemical components of Lilii Bulbus decoction， and to provide experimental support for the origin processing， decoction piece processing and clinical application of this herb. MethodUltra high performance liquid chromatography tandem quadrupole electrostatic field orbitrap high resolution mass spectrometry（UHPLC-Q-Orbitrap HRMS） was used for structural identification of the compounds using excimer ions， secondary MS and characteristic fragment ions， and referring to relevant literature and database information. Principal component analysis（PCA） and orthogonal partial least squares discriminant analysis（OPLS-DA） were used to screen the main differential components， the differential components were quantitatively studied by high performance liquid chromatography（HPLC）， in order to compare the types and contents of chemical components in the decoction of different processing products of Lilii Bulbus. ResultA total of 24 chemical components were identified from the decoction of different processed products of Lilii Bulbus， water extract and scalding liquid of fresh Lilii Bulbus， including 17 phenols， 5 saponins and 2 alkaloids. Compared with the fresh Lilii Bulbus decoction， the contents of regaloside A， p-coumaric acid， colchicine and other components in the decoction of dry Lilii Bulbus processed by scalding method decreased， the content of regaloside C in the decoction of dry Lilii Bulbus processed by steaming method decreased， and the contents of regaloside A and regaloside C in the decoction of fresh Lilii Bulbus processed by water immersion also decreased. Compared with the decoction of dry Lilii Bulbus processed by scalding method， the overall content of components in the fresh Lilii Bulbus decoction and the decoction of fresh Lilii Bulbus processed by water immersion was higher， the contents of components in the decoction of dry Lilii Bulbus processed by steaming method was higher， except for the slightly lower content of regaloside C. ConclusionDifferent processing processes have a certain effect on the types and contents of chemical components in Lilii Bulbus decoction. Scalding process is beneficial to the preservation of Lilii Bulbus， but can cause the loss of effective components. Compared with scalding method， steaming method can prevent browning of Lilii Bulbus and reduce the loss of its active ingredients. The processing method of removing foam after overnight immersion proposed by ZHANG Zhongjing may be more conducive to the treatment of Baihe disease， which can provide reference for the clinical rational application and mechanism research of different processed products of Lilii Bulbus.
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ObjectiveHigh performance liquid chromatography （HPLC） was used to establish the specific chromatograms of Aurantii Fructus from different origins， and the quality variability of Aurantii Fructus from Sichuan was analyzed and evaluated by combining entropy weighting method and grey correlation method. MethodHPLC was performed on an Agilent Eclipse Plus C18 column （4.6 mm×250 mm， 5 μm） with a gradient elution of methanol （A）-0.1% phosphoric acid aqueous solution as the mobile phase （0-12 min， 25%-33%A； 12-21 min， 33%-41%A； 21-30 min， 41%-42%A； 30-40 min， 42%-59%A； 40-53 min， 59%-72%A； 53-60 min， 72%A； 60-65 min， 72%-100%A； 65-70 min， 100%A； 70~71 min， 100%-25%A； 71-80 min， 25% A） at a flow rate of 1.0 mL·min-1， the injection volume was 10 μL and the detection wavelength was 330 nm. Fifty batches of Aurantii Fructus samples from different origins （Sichuan， Chongqing， Jiangxi and Hunan） were tested， and the similarity evaluation software is used to generate characteristic profiles and compare them with control profile for peak identification， and then to evaluate the similarity of the samples. IBM SPSS 19.0 and SIMCA 14.1 were used to perform multivariate statistical analysis on the results of the samples， and then the entropy weighting method and grey correlation were used to calculate the overall quality score of samples from Sichuan. ResultHPLC specific chromatogram of Aurantii Fructus was established， and 14 common peaks were identified as eriocitrin， neoeriocitrin， narirutin， naringin， hesperidin， neohesperidin， meranzin hydrate， poncirin， meranzin， marmin， nobiletin， 3，3′，4′，5，6，7，8-heptamethoxyflavone， tangeretin and auraptene. And the similarities between the samples from Sichuan and the control chromatogram were all above 0.980. The samples could be classified into four categories according to their main origins by chemical pattern recognition， and the results of cluster analysis， principal component analysis and orthogonal partial least squares-discriminant analysis were all able to discriminate the samples of different main origins effectively. The comprehensive evaluation results of entropy weighting method combined with grey correlation showed that the quality of Aurantii Fructus from Sichuan varied greatly among different origins， and the quality of Aurantii Fructus from Sichuan was ranked as Bazhong>Luzhou>Chongqing>Neijiang. ConclusionIn this study， the characteristic mapping of Aurantii Fructus from Sichuan is established， and combined with the analytical methods of chemometrics and grey correlation， the quality of samples from different origins can be effectively differentiated， which can provide a reference for the comprehensive evaluation and control of the quality of Aurantii Fructus from Sichuan.
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ObjectiveTo establish a high performance liquid chromatography（HPLC） fingerprint of Yanghetang benchmark sample， and evaluate its quality with chemometric methods， so as to provide a reference for the quality control of this benchmark sample. MethodHPLC was used to establish the fingerprint of Yanghetang benchmark sample with ZORBAX SB-C18 column（4.6 mm×250 mm， 5 μm）， the mobile phase was consisted of acetonitrile（A） -0.05% phosphoric acid aqueous solution （containing 0.05% triethylamine solution）（B） for gradient elution（0-5 min， 2%-3%A； 5-15 min， 3%-5%A； 15-65 min， 5%-30%A； 65-90 min， 30%-70%A）， the flow rate was 1.0 mL·min-1， the column temperature was 35 ℃， and the detection wavelength was 210， 260 nm. Traditional Chinese Medicine（TCM） Chromatographic Fingerprint Similarity Evaluation System （2012 edition） combined with cluster analysis， principal component analysis（PCA） and partial least squares-discriminant analysis（PLS-DA） were used to evaluate the quality differences between different batches of Yanghetang benchmark samples， and to find the main chemical components responsible for the quality differences. ResultHPLC fingerprint of Yanghetang benchmark sample was established， 13 common peaks were identified and attributed to each common peak， including peaks 2 and 8 from Rehmanniae Radix Praeparata， peaks 10 and 11 from Cinnamomi Cortex， peaks 1， 3-6 from fried Sinapis Semen， peak 13 from Ephedrae Herba， and peaks 7， 9， 12 from Glycyrrhizae Radix et Rhizoma. Eight of them were identified by comparing with control substance， which were 5-hydroxymethylfurfural（peak 2）， sinapine thiocyanate（peak 4）， glycyrrhizin（peak 7）， verbascoside（peak 8）， cinnamic acid（peak 10）， cinnamaldehyde（peak 11）， glycyrrhizic acid（peak 12） and ephedrine hydrochloride（peak 13）. The similarities of the HPLC fingerprints of 15 batches of Yanghetang benchmark samples with the control fingerprint were all greater than 0.80. The three chemometric methods could classify the samples into two categories. Eight differential components were screened out， among which 5-hydroxymethylfurfural， sinapine thiocyanate， verbascoside and ephedrine hydrochloride were identified. ConclusionThe established fingerprint analysis method is accurate， stable and reproducible， which basically reflects the overall chemical composition of Yanghetang benchmark sample， and can provide a basis for establishment of quality standards for compound preparations of this famous classical formula.
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Aromatic and medicinal plants are of great importance to determine the contents of the active compounds of plant origin and to evaluate them depending on variety and climate factors in order to determine the phenolic, antioxidant enzyme activity, vitamin contents in species belonging to the Lamiaceae family. Examination of the characteristics of different species, the highest peroxidase (POD) enzyme activity, ascorbate peroxidase (AxPOD), total antioxidant (TA), malondialdehyte (MDA), caffeic acids (CA), vitamin C contents,and chloric acid (ChA) were obtained in the M. longifoliaspecies. The highest vitamin E and catalase (CAT) were determined in the S. hortensisspecies but the highest total phenolic (TP), superoxide dismutase (SOD) enzyme, hydrogen peroxide (H2O2) and chlorogenic acid (ChgA) were determined in the S. spicigeraspecies. As a result of PCA analysis, it can be said that Mentha longifolia(L.) Hudson and Satureja spicigeraspecies have significant value in terms of biochemical and phenolic content.
Las plantas aromáticas y medicinales son de gran importancia para determinar el contenido de los compuestos activos de origen vegetal y evaluarlos en función de la variedad y factores climáticos con el fin de determinar la actividad enzimática fenólica, antioxidante, contenido vitamínico en especies pertenecientes a la familia Lamiaceae. El examen de las características de diferentes especies, la mayor actividad enzimática de peroxidasa (POD), ascorbato peroxidasa (AxPOD), antioxidante total (TA), malondialdehído (MDA), ácidos cafeicos (CA), contenido de vitamina C y ácido clorhídrico (ChA) se obtuvieron en la especie M. longifolia. La mayor cantidad de vitamina E y catalasa (CAT) se determinó en la especie S. hortensis, pero la mayor cantidad total de enzima fenólica (TP), superóxido dismutasa (SOD), peróxido de hidrógeno (H2O2) y ácido clorogénico (ChgA) se determinó en la especie S. spicigera. Como resultado del análisis de PCA, se puede decir que las especies Mentha longifolia(L.) Hudson y Satureja spicigeratienen un valor significativo en términos de contenido bioquímico y fenólico.
Subject(s)
Phenols/chemistry , Vitamins/chemistry , Lamiaceae/metabolism , Lamiaceae/chemistry , Antioxidants/chemistry , Plants, Medicinal/metabolism , Plants, Medicinal/chemistryABSTRACT
ObjectiveTo analyze changes of the chemical composition in Euodiae Fructus before and after processing with Coptidis Rhizoma decoction， so as to provide scientific basis for elucidating the processing mechanism of this decoction pieces. MethodUltra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry （UPLC-Q-TOF/MS） was performed on a Titank C18 column （2.1 mm×100 mm， 1.8 μm）， the mobile phase was 0.1% formic acid aqueous solution-acetonitrile for gradient elution， the column temperature was set at 40 ℃， the flow rate was 0.25 mL·min-1. Electrospray ionization （ESI） was used to scan in positive and negative ion modes， and the scanning range was m/z 50-1 250. The chemical constituents in Euodiae Fructus were identified before and after processing by reference substance comparison， database matching and literature reference， and MarkerView™ 1.2.1 software was used to normalize the obtained data， SIMCA-P 14.1 software was employed to perform principal component analysis （PCA） and orthogonal partial least squares-discriminant analysis （OPLS-DA） on MS data of raw and processed products to screen the differential components before and after processing. ResultA total of 50 compounds were identified， including 48 kinds of stir-fried products with Coptidis Rhizoma decoction and 44 kinds of raw products. After processing， six compounds were added， including danshensu， noroxyhydrastinine， oxyberberine， 13-methylberberrubine， protopine and canadine. However， two kinds of compounds， including （S）-7-hydroxysecorutaecarpine and wuchuyuamide Ⅱ， were not detected after processing. In general， after processing， the overall contents of phenolic acids and flavonoids decreased significantly， the overall content of limonoids increased， and the overall content of alkaloids did not decrease insignificantly. The results of PCA and OPLS-DA showed that there were significant differences in the composition and content of the chemical components of Euodiae Fructus before and after processing， and a total of 12 variables such as quercetin， dihydrorutaecarpine and dehydroevodiamine were obtained by screening. ConclusionEuodiae Fructus stir-fried with Coptidis Rhizoma decoction mainly contains phenolic acids， flavonoids， limonoids and alkaloids. The composition and content of the chemical components have some changes before and after processing. The addition of processing excipients and hot water immersion are the main reasons for the difference， which can provide experimental basis for interpretation of the processing mechanism of this characteristic processed products of Euodiae Fructus.
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ObjectiveTo analyze the flavor substances and change rules of Rhei Radix et Rhizoma during the process of nine-time repeating steaming and sun-drying. MethodThe flavor response values of Rhei Radix et Rhizoma samples were obtained by using PEN3 electronic nose system. The data were processed and analyzed by principal component analysis （PCA）， linear discriminant analysis （LDA） and Loadings analysis. ResultRhei Radix et Rhizoma processed with nine-time repeating steaming and sun-drying could be effectively distinguished into two categories as the sixth sample was the turning point. The samples steamed and dried for one to five times could be grouped into one category， the other four samples were obviously distinguished from them. The main flavor components reached the maximum response in the sample processed with six-time repeating steaming and sun-drying， and its response value of inorganic sulfur compounds was about 2.7 times that of the sample processed with one-time repeating steaming and sun-drying. In addition， compared with the raw products， the flavors of Rhei Radix et Rhizoma processed with nine-time repeating steaming and sun-drying and wine stewing changed significantly， and the response value of inorganic sulfur compounds in sample processed with nine-time repeating steaming and sun-drying was about 2.2 times that of raw products. From the perspective of flavor analysis， the response values of inorganic sulfur compounds and nitrogen-oxygen compounds in sample processed with nine-time repeating steaming and sun-drying were higher than those of wine-stewed products， and the two were not completely equivalent. ConclusionElectronic nose technology preliminarily clarifies the dynamic change rules of the flavor of Rhei Radix et Rhizoma during the process of nine-time repeating steaming and sun-drying from the flavor characteristics， and clarifies the difference between products processed with nine-time repeating steaming and sun-drying and wine-stewed products from the odor characteristics， which lays a foundation for revealing the processing principle of Rhei Radix et Rhizoma processed with nine-time repeating steaming and sun-drying.
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ObjectiveTo compare the effects of different drying methods on volatile components of Pseudostellariae Radix. MethodThe samples were dried by different methods， including air drying， sun drying， hot air drying （40， 60， 80 ℃） and vacuum freeze drying. Gas chromatography-ion mobility spectrometry （GC-IMS） was used to compare the changes of volatile components in the samples after different treatments. The samples were incubated at 80 ℃ and 500 r·min-1 for 15 min， the injection temperature was 85 ℃， the injection volume was 200 μL， the flow rate of carrier gas was from 2 mL to 150 mL during 20 min， and the temperature of IMS detector was 60 ℃. SE-54 capillary column （0.32 mm×30 m， 0.25 μm） was used， the column temperature was 60 ℃， and the analysis time was 35 min. The differential spectra of volatile components were constructed and analyzed by principal component analysis （PCA）. ResultA total of 37 volatile components were identified from dried Pseudostellariae Radix. The number of compounds in descending order was ketones， aldehydes and alcohols. There were some differences in the volatile components in samples dried by different methods. And the volatile components in samples with sun drying， air drying and hot air drying at 40 ℃ were similar， compared with other drying methods， vacuum freeze drying and hot air drying at 80 ℃ had great effects on the volatile components of Pseudostellariae Radix， and the compounds in the samples with vacuum freeze drying were the least. ConclusionIn this study， GC-IMS for the detection and analysis of volatile components in Pseudostellariae Radix is established， which has the characteristics of high efficiency， nondestructive inspection and simple sample processing. This method can be used for the distinction of Pseudostellariae Radix dried by different methods. And hot air drying at 40 ℃ can effectively retain the volatile components of Pseudostellariae Radix， and achieve similar flavor to samples with sun drying and air drying.
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Objective According to clinical demand of quantification evaluation on flat foot and high arch, an intelligent and rapid method to diagnose arch shape based on principal component analysis (PCA) of plantar pressure is proposed, and its clinic validity is tested. Methods Volunteers diagnozed as abnormal arch and healthy arch were included in this study, and a portable intelligent arch test system was designed and developed. By adopting thin-firm piezoresistive sensor array with 44 rows, 52 columns of sensing units, the system could collect plantar pressure distribution data from the subjects under static standing. Foot axis could be fitted automatically by using the self-programmed PCA, so that foot diagnosis was completed with diagnostic report. The plantar pressure results from the system were compared with those from the existing plantar pressure acquisition device, so as to verify precision of collected data. The accuracy of the diagnosis algorithm for flat foot, high arch and healthy foot was verified through comparison with clinical diagnosis. Results The result of the system had a good correlation with that of the existing plantar pressure acquisition device, the deviation of contact area acquired by the system was smaller than 3.2%, and the angle deviation of the fitted foot axis with clinically defined angel was less than 1°. The system was capable of making diagnosis on arch shape that was 92.6% consistent with the clinical diagnosis. Conclusions PCA is introduced to automatically fit foot axis to achieve the purpose of fast and accurate extraction of foot arch information. The method can be used to assist clinical diagnosis of flat foot and high arch foot, and contribute to quantative analysis on foot arch deformity and its pathogenesis study.
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ObjectiveA feedforward control model for dry granulation of polysaccharide components was established to guide the adjustment and optimization of critical process parameters （CPPs） in the design space， so as to reduce the impact of fluctuations in raw materials properties on the quality of medicines. MethodTaking Astragali Radix extract powder as the model drug， the design space of dry granulation CPPs was determined by Box-Behnken design. Astragali Radix mixed powder with different powder properties were prepared by mixture design， the variance inflation factor （VIF） was used to diagnose the multicollinearity of the powder properties， and principal component analysis （PCA） was used to extract the characteristic data of the model. Radial basis function neural network （RBFNN） was used to establish a feedforward control model for reflecting the relationship between the powder properties of polysaccharide components， dry granulation CPPs and one-time molding rate. ResultThe design space for dry granulation CPPs of polysaccharide components was 16-35 Hz for feeding speed， 10-23 Hz for roller speed， and 10-46 kg·cm-2 for roller pressure. The established RBFNN feedforward control model had a good predictive effect on the one-time molding rate of dry granulation of polysaccharide components， which could be used to guide the adjustment and optimization of CPPs in the design space， the relative error was 0.38%-6.73%， and the average relative error was 3.42%. ConclusionThe established feedforward control model can well reflect the relationship between the powder properties of the polysaccharide components， the dry granulation CPPs and the one-time molding rate of the granules， which can be used to guide the adjustment and optimization of CPPs in the design space， reduce the impact of material property fluctuation on product quality， and provide ideas for promoting the quality of traditional Chinese medicine from passive control to active control.
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ObjectiveBy comparing the composition and content changes of the volatile components in Atractylodis Rhizoma before and after processing with rice-washed water， the effect of rice-washed water processing on volatile components in Atractylodis Rhizoma was investigated. MethodHeadspace-gas chromatography-mass spectrometry （HS-GC-MS） was used to detect the volatile components in rhizomes of Atractylodes chinensis and A. lancea， and their processed products of rice-washed water. Chromatographic conditions were programmed temperature （starting temperature of 50 ℃ for 2 min， rising to 120 ℃ with the speed of 10 ℃·min-1， then rising to 170 ℃ at 2.5 ℃·min-1， and rising to 240 ℃ at 10 ℃·min-1 for 3 min）， the inlet temperature was 280 ℃， the split ratio was 10∶1， and the solvent delay time was 3 min. The conditions of mass spectrometry were electron bombardment ionization （EI） with ionization temperature at 230 ℃ and detection range of m/z 20-650. Then the relative content of each component was determined by the peak area normalization method. SIMCA 14.1 software was used to perform unsupervised principal component analysis （PCA） and supervised orthogonal partial least squares-discriminant analysis （OPLS-DA） on each sample data， the differential components of Atractylodis Rhizoma and its processed products were screened by the principle of variable importance in the projection （VIP） value>1. ResultA total of 60 components were identified， among which 40 were rhizomes of A. chinensis and 38 were its processed products， 46 were rhizomes of A. lancea and 47 were its processed products. PCA and OPLS-DA showed that the 4 kinds of Atractylodis Rhizoma samples were clustered into one category respectively， indicating that the volatile components of the two kinds of Atractylodis Rhizoma were significantly changed after processing with rice-washed water， and there were also significant differences in the volatile components of rhizomes of A. lancea and A. chinensis. The compound composition of Atractylodis Rhizoma and its processed products was basically the same， but the content of the compounds was significantly different. The differential components were mainly concentrated in monoterpenoids and sesquiterpenoids， and the content of monoterpenoids mostly showed a decreasing trend. ConclusionAfter processing with rice-washed water， the contents of volatile components in rhizomes of A. lancea and A. chinensis are significantly changed， and pinene， 3-carene， p-cymene， ocimene， terpinolene， atractylon， acetic acid and furfural can be used as difference markers before and after processing.
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ObjectiveTo identify the chemical constituents of Alismatis Rhizoma before and after processing with salt-water by ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry （UPLC-Q-TOF-MS）， and to investigate the changes of terpenoids in Alismatis Rhizoma before and after processing with salt-water. MethodUPLC-Q-TOF-MS was used to detect with 0.1% formic acid aqueous solution （A）-acetonitrile （B）as mobile phase for gradient elution （0-0.01 min， 20%B； 0.01-5 min， 20%-40%B； 5-40 min， 40%-95%B； 40-42 min， 95%B； 42-42.1 min， 95%-20%B； 42.1-45 min， 20%B）， electrospray ionization （ESI） was selected for collection and detection in positive ion mode with the scanning range of m/z 100-1 250 and ion source temperature at 500 ℃. The data were analyzed by PeakView 1.2.0.3， the components were identified according to the primary and secondary MS data， and combined with the reference substance and literature. After normalized treatment by MarkerView 1.2.1， the MS data were analyzed by principal component analysis （PCA） and orthogonal partial least squares-discriminant analysis （OPLS-DA）， and then the differential components before and after processing were screened. The content changes of differential components were analyzed according to the relative peak area. ResultA total of 30 components were identified under positive ion mode， including 28 prototerpene triterpenes and 2 sesquiterpenes. The results of PCA and OPLS-DA showed that there were significant differences in components from Alismatis Rhizoma before and after processing with salt-water， and 10 differential components （alisol B 23-acetate， alisol I， alismol， 11-deoxy-alisol B 23-acetate， alisol B， alisol C， 11-deoxy-alisol B， alisol G， 11-deoxy-alisol C and alisol A） were screened， and the contents of alisol G and alisol A decreased significantly after processing. ConclusionUPLC-Q-TOF-MS can comprehensively and accurately identify the chemical constituents in raw and salt-processed products of Alismatis Rhizoma. It takes a great difference in the contents of chemical constituents before and after processing， and the difference of substituents is the main reason for this differences， which can provide reference for determining the material basis of efficacy changes of Alismatis Rhizoma before and after processing with salt-water.
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ObjectiveTo identify the chemical constituents of Alismatis Rhizoma before and after processing with salt-water by ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry （UPLC-Q-TOF-MS）， and to investigate the changes of terpenoids in Alismatis Rhizoma before and after processing with salt-water. MethodUPLC-Q-TOF-MS was used to detect with 0.1% formic acid aqueous solution （A）-acetonitrile （B）as mobile phase for gradient elution （0-0.01 min， 20%B； 0.01-5 min， 20%-40%B； 5-40 min， 40%-95%B； 40-42 min， 95%B； 42-42.1 min， 95%-20%B； 42.1-45 min， 20%B）， electrospray ionization （ESI） was selected for collection and detection in positive ion mode with the scanning range of m/z 100-1 250 and ion source temperature at 500 ℃. The data were analyzed by PeakView 1.2.0.3， the components were identified according to the primary and secondary MS data， and combined with the reference substance and literature. After normalized treatment by MarkerView 1.2.1， the MS data were analyzed by principal component analysis （PCA） and orthogonal partial least squares-discriminant analysis （OPLS-DA）， and then the differential components before and after processing were screened. The content changes of differential components were analyzed according to the relative peak area. ResultA total of 30 components were identified under positive ion mode， including 28 prototerpene triterpenes and 2 sesquiterpenes. The results of PCA and OPLS-DA showed that there were significant differences in components from Alismatis Rhizoma before and after processing with salt-water， and 10 differential components （alisol B 23-acetate， alisol I， alismol， 11-deoxy-alisol B 23-acetate， alisol B， alisol C， 11-deoxy-alisol B， alisol G， 11-deoxy-alisol C and alisol A） were screened， and the contents of alisol G and alisol A decreased significantly after processing. ConclusionUPLC-Q-TOF-MS can comprehensively and accurately identify the chemical constituents in raw and salt-processed products of Alismatis Rhizoma. It takes a great difference in the contents of chemical constituents before and after processing， and the difference of substituents is the main reason for this differences， which can provide reference for determining the material basis of efficacy changes of Alismatis Rhizoma before and after processing with salt-water.
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ObjectiveBy comparing the composition and content changes of the volatile components in Atractylodis Rhizoma before and after processing with rice-washed water， the effect of rice-washed water processing on volatile components in Atractylodis Rhizoma was investigated. MethodHeadspace-gas chromatography-mass spectrometry （HS-GC-MS） was used to detect the volatile components in rhizomes of Atractylodes chinensis and A. lancea， and their processed products of rice-washed water. Chromatographic conditions were programmed temperature （starting temperature of 50 ℃ for 2 min， rising to 120 ℃ with the speed of 10 ℃·min-1， then rising to 170 ℃ at 2.5 ℃·min-1， and rising to 240 ℃ at 10 ℃·min-1 for 3 min）， the inlet temperature was 280 ℃， the split ratio was 10∶1， and the solvent delay time was 3 min. The conditions of mass spectrometry were electron bombardment ionization （EI） with ionization temperature at 230 ℃ and detection range of m/z 20-650. Then the relative content of each component was determined by the peak area normalization method. SIMCA 14.1 software was used to perform unsupervised principal component analysis （PCA） and supervised orthogonal partial least squares-discriminant analysis （OPLS-DA） on each sample data， the differential components of Atractylodis Rhizoma and its processed products were screened by the principle of variable importance in the projection （VIP） value>1. ResultA total of 60 components were identified， among which 40 were rhizomes of A. chinensis and 38 were its processed products， 46 were rhizomes of A. lancea and 47 were its processed products. PCA and OPLS-DA showed that the 4 kinds of Atractylodis Rhizoma samples were clustered into one category respectively， indicating that the volatile components of the two kinds of Atractylodis Rhizoma were significantly changed after processing with rice-washed water， and there were also significant differences in the volatile components of rhizomes of A. lancea and A. chinensis. The compound composition of Atractylodis Rhizoma and its processed products was basically the same， but the content of the compounds was significantly different. The differential components were mainly concentrated in monoterpenoids and sesquiterpenoids， and the content of monoterpenoids mostly showed a decreasing trend. ConclusionAfter processing with rice-washed water， the contents of volatile components in rhizomes of A. lancea and A. chinensis are significantly changed， and pinene， 3-carene， p-cymene， ocimene， terpinolene， atractylon， acetic acid and furfural can be used as difference markers before and after processing.
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Objective To develop an SNP Panel for East Asian population, which has a high individual identification rate and the capability of ancestry analysis. Methods The 55 SNP Panel by Professor KIDD of Yale University and the 128 SNP Panel by Professor SELDIN of Davis School of California University, 170 SNP Panel in total was used as the basis and its test data in the East Asian population was collected. The genetic parameters of SNP loci were calculated and combined with the results of heatmap analysis to screen SNP loci suitable for East Asian population. Some Tibetan and Han samples were tested. The possibility of using the SNP loci in ancestry inference was analyzed by means of STRUCTURE analysis, principal component analysis and heatmap analysis. Results A Panel with 45 SNPs （45 SNP Panel） was screened out, and the average genetic parameters of each SNP were better than 170 SNP Panel, with the same ancestry analysis and inference ability. Conclusion In terms of ancestry inference information, the 45 SNP Panel can completely replace the 170 SNP Panel and achieve the same ancestry analysis and inference ability. In genetic parameters, 45 SNP Panel is better than 170 SNP Panel in the East Asian population, which shows its important potential forensic application value.
Subject(s)
Humans , Asian People/genetics , Gene Frequency , Genetics, Population , Polymorphism, Single Nucleotide , Principal Component AnalysisABSTRACT
Objective To establish the three-dimensional (3D) statistical shape model (SSM) of the foot, so as to reveal the 3D foot shape variations. Methods Foot data from 50 normal Chinese young males were used for 3D statistical shape modelling. Steps, including mesh registration of foot surface, axis alignment and principal component (PC) analysis (dimension reduction), were performed to obtain the parameterized foot shape (mean shape and standard deviation of PC). Results Through the principal component analysis (PCA), the 3D foot shape varied in the length and width (PC1, 48.01%), arch and dorsal height (PC2, 11.38%), and hallux abduction-adduction position (PC3, 7.48%). Conclusions Based on the parameterised 3D foot SSM, these datasets can be applied into the population-based shoe last manufacture, orthotics customization and quick diagnosis of foot disorders in clinic.
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Objective:To establish the ultraperformance liquid chromatography （UPLC） fingerprint of Pipa Qingfeiyin substance benchmark， and to establish a quantitative analysis method for simultaneous determination of the contents of five index components， so as to provide reference for the quality control and evaluation of this famous classical formula. Method:ACQUITY UPLC<sup>®</sup> CSH<sup>TM</sup> C<sub>18</sub> column （2.1 mm×100 mm， 1.7 μm） was used with mobile phase of acetonitrile （A）-0.1% formic acid aqueous solution （B） for gradient elution （0-7 min， 5%-7%A； 7-11 min， 7%-8%A； 11-22 min， 8%-14%A； 22-30 min， 14%-15%A； 30-35 min， 15%-25%A； 35-42 min， 25%-40%A； 42-45 min， 40%-50%A； 45-50 min， 50%-60%A）， the flow rate was 0.35 mL·min<sup>-1</sup>， the column temperature was 25 ℃， the detection wavelengths were 278 nm and 248 nm. UPLC fingerprints of 15 batches of Pipa Qingfeiyin substance benchmark were established， and the "Similarity Evaluation System of Chromatographic Fingerprint of Traditional Chinese Medicine" software （2012 edition） was used for similarity analysis， and the common peaks were assigned. Cluster analysis （CA）， principal component analysis （PCA） and orthogonal partial least squares discriminant analysis （OPLS-DA） were used to evaluate the fingerprint data. UPLC fingerprint method was used to simultaneously determine the contents of five components in the substance benchmark. Result:The method validation of fingerprint and determination method was good， the similarities between 15 batches of Pipa Qingfeiyin substance benchmark and their control fingerprint were ≥0.997， 23 common peaks were identified and 11 chromatographic peaks were identified. CA， PCA and OPLS-DA divided 15 batches of the substance benchmark into two groups. The linear relationship of phellodendrine hydrochloride， chlorogenic acid， berberine hydrochloride， palmatine hydrochloride and ammonium glycyrrhizinate was good in a certain range of concentration （<italic>R</italic><sup>2</sup>>0.999）， their average recovery was 96.47%-101.16%， and the contents of these five components in the substance benchmark were 0.87-2.00， 1.53-5.95， 18.45-33.97， 3.87-6.29， 1.02-4.12 mg·g<sup>-1</sup>， respectively. Conclusion:The established UPLC fingerprint and multi-index component content determination methods have strong specificity， good resolution and high sensitivity， it can be characterized except for the Ginseng Radix et Rhizoma flavor， which can provide reference for the quality control and evaluation of Pipa Qingfeiyin compound preparation.
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Objective:Based on pharmacokinetics， the antitussive and expectorant related quality markers （Q-marker） of Trichosanthis Fructus were screened from diosmetin-7-<italic>O</italic>-glucopyranoside， diosmetin， apigenin， vanillic acid and cinnamic acid， and the candidate Q-marker was evaluated by multivariate statistical method. Method:Six healthy rats were randomly selected and the 70% ethanol extract of Trichosanthis Fructus （dose of 20 g·kg<sup>-1</sup>） was given by intragastric administration. Blood was collected from the orbital vein at different time points， and the plasma concentrations of 5 components （diosmetin-7-<italic>O</italic>-glucopyranoside， diosmetin， apigenin， vanillic acid and cinnamic acid） from Trichosanthis Fructus were detected simultaneously by high performance liquid chromatography-triple quadrupole tandem mass spectrometry （HPLC-QqQ-MS/MS）. The main detection conditions were as following：mobile phase of 0.2% formic acid aqueous solution （A）-acetonitrile （B） for gradient elution （0-4 min， 6%-23%B； 4-5 min， 23%-59.5%B； 5-10 min， 59.5%-60%B）， flow rate of 0.5 mL·min<sup>-1</sup>， the detection wavelength at 254 nm， electrospray ionization （ESI）， positive ion mode detection， multiple reaction monitoring （MRM） mode scanning， scanning range of <italic>m</italic>/<italic>z</italic> 50-1 500. Diosmetin-7-<italic>O</italic>-glucopyranoside， diosmetin， apigenin and vanillic acid with clear pharmacokinetic behaviors were selected as candidate Q-marker about antitussive and expectorant of Trichosanthis Fructus. The contents of these components in 9 batches of medicinal materials were determined and the main detection conditions were the same as the pharmacokinetic study. SPSS 21.0 was used for cluster analysis and principal component analysis （PAC） based on the results of determination. Result:The pharmacokinetic results showed that the area under concentration-time curve （AUC<sub>0-</sub><italic><sub>t</sub></italic>） of 4 components （diosmetin-7-<italic>O</italic>-glucopyranoside， diosmetin， apigenin and vanillic acid） were （111.28±9.94）， （27.08±2.76）， （1 376.12±101.86）， （631.32±64.72） μg·h·L<sup>-1</sup>， respectively. The 9 batches of Trichosanthis Fructus samples were clustered into 3 groups by systematic cluster analysis. The clustering results were related to the variety of Trichosanthis Fructus and also affected by the origin. The PCA results showed that the comprehensive scores of Gaotang Trichosanthis Fructus， Shanxi Trichosanthis Fructus， Hebei Ben Trichosanthis Fructus were 1.919， 1.356 and 0.299， respectively， ranking in the top 3 among all samples. The comprehensive scores of Nongkeyuan No. 1， Hebei Trichosanthis Fructus and Nongkeyuan No. 2 were -0.804， -1.085， -1.120， respectively， which were in the last 3 positions among all samples. Conclusion:The pharmacokinetic characteristics and quality evaluation of diosmetin-7-<italic>O</italic>-glucopyranoside， diosmetin， apigenin and vanillic acid meet the requirements about antitussive and expectorant related Q-marker of Trichosanthis Fructus.
ABSTRACT
Objective:To establish the high performance liquid chromatography （HPLC） fingerprint of Citri Sarcodactylis Fructus， and to search for makers to characterize the quality difference of Citri Sarcodactylis Fructus from different origins coupled with chemometrics. Method:The analysis was performed on a Thermo Hypersil GOLD C<sub>18</sub> column （4.6 mm×250 mm， 5 μm） with mobile phase consisted of acetonitrile-0.05% phosphoric acid solution for gradient elution， and the detection wavelength was set at 254 nm. A total of 31 batches of samples were analyzed to establish the HPLC fingerprint of Citri Sarcodactylis Fructus. Similarity evaluation was performed by Traditional Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System （2012 edition） to confirm the common peaks， which were identified by comparison of reference substances. On the basis， chemometrics methods were used to analyze and evaluate the quality of Citri Sarcodactylis Fructus from different origins. At the same time， 3 batches of 5 species of decoction pieces from the genus <italic>Citrus</italic> in the family Rutaceae， including Citri Sarcodactylis Fructus， Aurantii Fructus Immaturus， Aurantii Fructus， Citri Reticulatae Pericarpium Viride and Citri Reticulatae Pericarpium， were randomly collected for evaluating the effectiveness and reliability of the established HPLC fingerprint of Citri Sarcodactylis Fructus. Result:HPLC fingerprint of Citri Sarcodactylis Fructus was established and 22 common peaks were identified. And seven common peaks among them were identified as 6，7-dimethoxycoumarin， diosmin， hesperidin， byakangelicin， 5，7-dimethoxycoumarin， bergapten and oxypeucedanin. Except for 2 batches of samples， the similarities of fingerprints between other 29 batches of samples were >0.9. The 31 batches of Citri Sarcodactylis Fructus were basically divided into 3 groups by cluster analysis and principal component analysis， which were consistent with the classification of three different producing areas. Eight differential markers were screened by orthogonal partial least squares discriminant analysis and four of them （5，7-dimethoxycoumarin， bergapten， 6，7-dimethoxycoumarin and diosmin） were identified by reference substances. Similarity evaluation of 5 species of decoction pieces from genus <italic>Citrus</italic> in the family Rutaceae was carried out by taking the reference fingerprint of Citri Sarcodactylis Fructus as treference chromatogram， similarity of Citri Sarcodactylis Fructus decoction pieces was 0.892-0.977， and the similarities of the other 4 kinds of decoction pieces were 0.215-0.517. Conclusion:The established fingerprint method is reasonable， effective and accurate for quality control of Citri Sarcodactylis Fructus， the characterization information is more comprehensive combined with chemometrics.