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1.
Article in Chinese | WPRIM | ID: wpr-879046

ABSTRACT

The extract rates, multicomponent content and fingerprint were determined in this study to investigate the quality diffe-rence between standard decoction of raw Paeoniae Radix Alba and fried Paeoniae Radix Alba. UPLC fingerprint was established for 17 batches of standard decoction of raw and fried Paeoniae Radix Alba, and the contents of gallic acid, catechin, albiflorin, paeoniflorin and benzoyl paeoniflorin were determined. The peak areas of standard decoction were analyzed by the independent t-test and orthogonal partial least squares discriminant analysis. There was no significant difference in extract rates between the standard decoction of raw and fried Paeoniae Radix Alba. After fried processing, the content of albiflorin increased by 0.26%, while the contents of gallic acid, catechin, paeoniflorin and benzoyl paeoniflorin decreased by 13.04%, 27.97%, 10.30% and 18.79% respectively. There were 14 common peaks in the fingerprint of standard decoction of raw Paeoniae Radix Alba, and 16 common peaks in the fried Paeoniae Radix Alba. Peak 1 and peak 3 were new ones after processing, among which the peak 3 was 5-hydroxymethylfurfural. The results showed that peak 1, peak 3, peak 11 and peak 15 were the key compounds to distinguish standard decoction of raw and fried Paeoniae Radix Alba. In conclusion, this method is stable and can be used for the study of quantity transfer and quality control in the preparation process of standard decoction, granules and other dosage forms for raw and fried Paeoniae Radix Alba, providing reference for the identification of raw and fried Paeoniae Radix Alba and related preparations.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Paeonia , Quality Control , Reference Standards
2.
Article in Chinese | WPRIM | ID: wpr-906325

ABSTRACT

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.

3.
Article in Chinese | WPRIM | ID: wpr-905972

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.

4.
Article in Chinese | WPRIM | ID: wpr-873079

ABSTRACT

Objective::To develop high performance liquid chromatography-diode array detector (HPLC-DAD) wavelength switching for simultaneously determining the contents of inosine, loganic acid, chlorogenic acid, amygdalin, hydroxysafflor yellow A, gentiopicroside, ferulic acid and liquiritin in 15 batches of material benchmarks of Shentong Zhuyutang. Method::The quantitative analysis was carried out on a Thermo Hypersil GOLD C18 column (4.6 mm×250 mm, 5 μm) with mobile phase of acetonitrile-0.1%phosphoric acid aqueous solution for gradient elution, the flow rate was 1.0 mL·min-1, the detection wavelengths were set as 248 nm (0-11 min, inosine), 235 nm (11-14 min, loganic acid), 324 nm (14-16 min, chlorogenic acid), 220 nm (16-19 min, amygdalin and hydroxysafflor yellow A), 274 nm (19-26 min, gentiopicroside), 247 nm (26-54 min, ferulic acid and liquiritin), the column temperature was maintained at 25 ℃. According to the contents of eight active components in 15 batches of material benchmarks, orthogonal partial least squares discriminant analysis (OPLS-DA) in SIMCA 14.1 was used to evaluate the quality difference of each batch of samples. Result::Each component had good separations, the linear ranges of the above 8 components were 2.1-67.2, 1.812 5-58, 1.937 5-62, 5.212 5-166.8, 8.45-270.4, 7.075-226.4, 1.775-56.8, 3.875-124 mg·L-1, respectively (r≥0.999 6). The average recoveries of them were 99.23%, 100.09%, 99.33%, 98.85%, 99.15%, 98.75%, 99.42%, 98.96%, respectively (RSD<2%). The contents of the above eight components in 15 batches of material benchmarks were 0.183 5-0.250 3, 0.173 1-0.265 3, 0.069 5-0.169 8, 0.959 2-1.458 2, 1.905 4-2.553 3, 0.933 3-1.997 5, 0.084 6-0.143 4, 0.212 5-0.704 3 mg·g-1, respectively. Liquiritin, ferulic acid, gentiopicroside and hydroxysafflor yellow A were determined to have significant impact on the quality of different batches of material benchmarks of Shentong Zhuyutang through OPLS-DA. Conclusion::The established method for simultaneous determination of multi-components is reliable, simple and in line with the requirements of methodological verification. It is suitable for the quality control of research and development of compound preparations of Shentong Zhuyutang.

5.
Article in Chinese | WPRIM | ID: wpr-873030

ABSTRACT

Objective:To improve the quality standard of Shenwei Gubi tablets, and to explore the reasons for the great difference in the contents of quality control index components between batches of this product. Method:The fingerprint of this product was established by HPLC, the determination was performed on Diamonsil C18 column (4.6 mm×250 mm, 5 μm) with acetonitrile (A)-0.1% phosphoric acid solution (B) for gradient elution (0-5 min, 10%A; 5-15 min, 10%-12%A; 15-30 min, 12%-26%A; 30-43 min, 26%-31%A, 43-50 min, 31%-40%A, 50-70 min, 40%-55%A; 70-84 min, 55%-72.5%A) as the mobile phase at detection wavelength of 230 nm. The orthogonal partial least squares-discriminant analysis-variable importance in the projection (OPLS-DA-VIP) map was drawn with the common peak as the independent variable. The contribution of 26 common peaks to the fingerprint differences among different batches of this product was quantified. By searching for the chromatographic peaks with great differences, combined with relevant literature, the components related to the clinical indications of the product were screened out and their contents were determined by specificity experiment, and the quantitative indicators were finally selected. HPLC-doide array detector (DAD) was employed to determine the contents of the above preferred indexes with detection wavelengths of 236, 276, 230, 322 nm, other conditions were the same as HPLC fingerprint detection method. Result:A total of 26 common peaks were calibrated on the HPLC fingerprint of Shenwei Gubi tablets. The similarity between the fingerprint of each batch samples and the reference fingerprint was≥0.950. Loganic acid, gentiopicroside, paeoniflorin and osthole were optimized as the quantitative indicators of this product, their average contents were 161.02, 401.80, 255.54, 80.68 μg·g-1. Conclusion:The established fingerprint and multi-index quantitative analysis method are stable and reliable, and can be used for quality control of Shenwei Gubi tablets. Difference in contents of quality control components between batches of raw materials and the imperfect quality control method of intermediates in the production process are the main reasons for the great difference in the contents of quality control indicators between batches of this product.

6.
Article in Chinese | WPRIM | ID: wpr-827999

ABSTRACT

This work is to establish the fingerprint of Astragalus membranaceus var. mongholicus by HPLC-ELSD method, and to analyze the simulated wildness degree of A. membranaceus var. mongholicus in the genuine region of Inner Mongolia, Ningxia and Gansu. Compared with wild A. membranaceus var. mongholicus, the quality differences of A. membranaceus var. mongholicus in the genuine region were analyzed by identification of chromatographic peaks and similarity evaluation, cluster analysis(CA), principal components analysis(PCA) and orthogonal partial least squares discriminant analysis(OPLS-DA). HPLC fingerprints of A. membranaceus var. mongholicus in different genuine regions are established. The qualitative analysis of mass spectrometry identified 18 components. The similarity evaluation shows that the similarity of 32 batches of A. membranaceus var. mongholicus samples was 0.688-0.993. Among them, the similarity of samples in Shanxi, Inner Mongolia, Ningxia is 0.688-0.993, 0.835-0.989, 0.934-0.988, respectively and the similarity of samples in Gansu is 0.729-0.876 except No. 25 sample. The results of CA show that the samples of A. membranaceus var. mongholicus can be grouped into four categories according to the production area except the No. 11 and No. 25 samples. The results of PCA indicate that 32 batches of A. membranaceus var. mongholicus samples can be clustered according to quality and origin, and the quality of A. membranaceus var. mongholicus in Inner Mongolia is the closest to the wild breed. The results of OPLS-DA indicate that there are six components that can distinguish the wild and domestic A. membranaceus var. mongholicus, which are malonylastragaloside Ⅰ, astragaloside Ⅰ, calycosin-7-O-β-D-glycoside-6″-O-malonate, calycosin-7-O-β-D-glycoside, formononetin-7-O-β-D-glycoside-6″-O-malonate, and astrapterocarpan-3-O-β-D-glycoside-6″-O-malonate. The established method can be used to analyze differences between A. membranaceus var. mongholicus origin and planting environment, and can provide references for the protection and replacement of wild A. membranaceus var. mongholicus resources, and the cultivation, processing and production of A. membranaceus var. mongholicus.


Subject(s)
Astragalus propinquus , China
7.
Article in Chinese | WPRIM | ID: wpr-846367

ABSTRACT

Objective: To identify and comprehensively evaluate Cynomorium songaricum from different producing areas in order to provide reference for the quality evaluation of C. songaricum and the determination of the suitability of the origin. Methods: A total of 40 samples from five provinces (regions) were collected to measure the content of gallic acid, protocatechuic acid, catechins, total polysaccharides, total flavonoids, Na, K, Ca, Mg, Fe, Zn, Mn, Co, Sr, Ni, Ag, Ba, Ti, Cu, Pb, Cr, Cd, As, and Hg. The data reflecting the quality of C. songaricum were analyzed by orthogonal partial least squares discriminant analysis (OPLS-DA) and entropy weight TOPSIS analysis. Results: The contents of Mn, Zn, Co, catechin, Pb, Cr, Ca, Ti, total flavonoids, protocatechuic acid, Mg and Cu in C. songaricum are important for distinguishing different producing areas. The quality of C. songaricum in Inner Mongolia was the best in all provinces (regions), followed by Gansu, Ningxia, Xinjiang, and Qinghai Provinces. Conclusion: The results of OPLS-DA combined with entropy weight TOPSIS analysis are reasonable, objective and effective, and can be applied to the comprehensive evaluation of multiple indicators of C. songaricum.

8.
Article in Chinese | WPRIM | ID: wpr-846205

ABSTRACT

Objective: To compare the difference of volatile specific odor components of Angelicae Sinensis Radix (ASR) processed by different methods such as yellow wine washing, dipping and firing, so as to provide research ideas for establishing the identification methods of different processed products of ASR and further study the mechanism of ASR traditional methods. Methods: Gas chromatography-ion mobility spectrometry (GC-IMS) was used to detect and compare the volatile components of ASR samples washed with different concentrations and processed by different methods, and compare the composition changes. PCA, partial least squares discriminant analysis (PLS-DA), and orthogonal partial least squares discriminant analysis (OPLS-DA) were used to analyze the differences in volatile components combined with SIMCA 14.1 software. Results: GC-IMS fingerprints showed that the volatile components of ASR at different concentrations were different. It was identified that the volatile components included 55 monomers and dimers and polymers of some substances. 2-Octanol, E-2-heptan aldehydes, acetone, 2-pentanone and 5-methyl-2-furan methanol could be used as the characteristic volatile substances of yellow wine washing of ASR. Ethyl acetate, 3-methyl-1-pentanol, 2-hexanol and ethyl 2-methylbutyrate could be used as characteristic flavor substances of yellow wine dipping of ASR. Furfural dimer, 3-methylbutanol and benzaldehyde could be used as characteristic volatile substances of yellow wine firing of ASR. The results of PCA showed that the resolution of each group of samples was good. PLS-DA analysis showed that 2-undecenal, 2-butanone, and acetone were different components with different concentrations yellow wine washing of ASR samples. OPLS-DA analysis showed that 2-undecenal, ethyl octanoate, dimer and acetone were the main components of ASR samples processed by different methods. Conclusion: The GC-IMS technology combined with stoichiometry proved that the volatile components of ASR processed by yellow wine washing, dipping and firing were different, which provided a reference for further research on traditional processing methods in classical prescription.

9.
Article in Chinese | WPRIM | ID: wpr-850771

ABSTRACT

Objective: To establish the fingerprint chromatography of Shujin Huoxue products (Shujin Huoxue Capsule and Shujin Huoxue Tablet) and provide a reference for its overall quality evaluation. Methods: The analysis was performed on Agilent Poroshell 120 SB-C18 (150 mm × 4.6 mm, 2.7 μm) column with acetonitrile-0.2% formic acid solution for gradient elution, the flow rate was 0.5 mL/min, the detection wavelength was 277 nm, and the column temperature was 30 oC. HPLC of 23 batches of Shujin Huoxue products were analyzed by the software “Similarity Evaluation System for Chromatographic Fingerprint of TCM (2012 edition)” combined with principal component analysis (PCA), cluster analysis (CA), and orthogonal partial least squares discriminant analysis (OPLS-DA). Results: The similarity of 18 batches (S1-S17 and S23) of samples was more than 0.900, 23 batches of samples could be clustered into three groups by PCA, CA, and OPLS-DA analysis. Among these, S1-S16 were clustered into group I, S23 and S17 could be divided into group II, and S18-S22 were clustered into group III. Four common peaks with larger differences were determined from 10 common peaks, including peaks 1, 3 (5-hydroxymethylfurfural), 6 (phenylacetic acid), and 10 (4-methoxy salicylaldehyde). Conclusion: Fingerprint chromatography combined with chemical pattern recognition technique was stable and simple, which could be used to evaluate the quality of Shujin Huoxue products systematically and comprehensively.

10.
Article in Chinese | WPRIM | ID: wpr-850698

ABSTRACT

Objective: To establish the fingerprints of nucleosides in Cervi Cornu Pantotrichum (CCP) pieces by HPLC method, perform cluster analysis and principal component analysis (PCA), and compare the differences of six nucleosides in CCP pieces. Methods: A total of 16 batches of CCP pieces from different origins were determined by HPLC. Sixteen batches from different origins in China were collected to assess the similarities according to similarity evaluation for “chromatographic fingerprint of traditional Chinese medicine” (2012), and four kinds of decoction pieces were distinguished and compared by chemometric methods such as principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA). Results: The HPLC fingerprints of CCP nucleosides were established and the similarity was above 0.960. Six common peaks of uracil, adenine, hypoxanthine, uridine, inosine, and guanosine were identified. Among them, uracil, hypoxanthine, and inosine were different compounds, which can be used as a quality control indicator for identifying and distinguishing CCP pieces. Conclusion: The CCP nucleoside fingerprints established by the method are characterized by strong features and simple methods. The combination of six nucleosides can better control the quality, which has guiding significance and reference value for the identification and quality control of CCP.

11.
Acta Pharmaceutica Sinica B ; (6): 157-166, 2019.
Article in English | WPRIM | ID: wpr-774994

ABSTRACT

Pharmacometabolomics has been already successfully used in toxicity prediction for one specific adverse effect. However in clinical practice, two or more different toxicities are always accompanied with each other, which puts forward new challenges for pharmacometabolomics. Gastrointestinal toxicity and myelosuppression are two major adverse effects induced by Irinotecan (CPT-11), and often show large individual differences. In the current study, a pharmacometabolomic study was performed to screen the exclusive biomarkers in predose serums which could predict late-onset diarrhea and myelosuppression of CPT-11 simultaneously. The severity and sensitivity differences in gastrointestinal toxicity and myelosuppression were judged by delayed-onset diarrhea symptoms, histopathology examination, relative cytokines and blood cell counts. Mass spectrometry-based non-targeted and targeted metabolomics were conducted in sequence to dissect metabolite signatures in predose serums. Eventually, two groups of metabolites were screened out as predictors for individual differences in late-onset diarrhea and myelosuppression using binary logistic regression, respectively. This result was compared with existing predictors and validated by another independent external validation set. Our study indicates the prediction of toxicity could be possible upon predose metabolic profile. Pharmacometabolomics can be a potentially useful tool for complicating toxicity prediction. Our findings also provide a new insight into CPT-11 precision medicine.

12.
Chinese Pharmacological Bulletin ; (12): 833-839, 2019.
Article in Chinese | WPRIM | ID: wpr-857235

ABSTRACT

Aim: To evaluate the mouse model of hypertriglyceridemia (hTG) induced by schisandrin B (Sch B) using lipid metabolomics technology. Methods: Male ICR mice weighing 23 ~ 27 g were randomly divided into four groups: (1) mice fed with normal diet (ND group) (2) mice fed with ND and treated with Sch B(ND +Sch B group); (3) mice fed with high fat/fructose diet(HFFD group; fat, 10%; fructose, 10%; w/w), and (4) mice fed with HFFD and treated with Sch B (HFFD + Sch B group). Based on our previous research, Sch B at a single dose of 2 g · kg-1 was orally administered to the animals in the current study. Forty-eight hours later, serum samples were obtained from the orbital vein. Serum triglyceride (TG) and total cholesterol (TC) were analyzed by biochemical method. The metabolic fingerprint spectrum of serum in all groups were obtained and analyzed using ultra-performance liquid chromatography quadrupole-time-of-flight mass spectrometry (UPLC-Q/TOF-MS) method. The differences of metabolic spectra in every two groups were compared via the multivariate statistical methods. Results: Compared with ND group, three kinds (27 markers) of differential metabolites were identified in ND +Sch B group, including 18 TG, 7 phosphatidylcholine (PC), and 2 phosphatidylethano-lamine(PE). Compared with ND group, five kinds(27 markers) of differential metabolites were screened in HFFD group, including 6 sphingomyelin (SM), 13 PC, 2 cholesteryl ester(CE), 5 TG and 1 phosphati-dylinositol (PI). Compared with HFFD group, four kinds (25 markers) of differential metabolites were found in HFFD + Sch B group, involving 14 TG, 1 CE, 6 PC and 4 PE. Conclusion: These findings suggest that the animal model of hypertriglyceridemia established by Sch B involves the alteration of serum lipid metabolomics.

13.
Article in Chinese | WPRIM | ID: wpr-838078

ABSTRACT

Objective: To explore the surface-enhanced Raman spectroscopy (SERS) difference of key female fertility indicators, estradiol (E2), anti-Müllerian hormone (AMH) and antral follicle count (AFC) in serum samples of healthy and infertile women, and the possibility of their application in preliminary screening of clinical female fertility. Methods: A total of 236 serum samples of healthy and infertile women of childbearing age were collected from Reproductive Medical Center of the First Affliated Hospital with Nanjing Medical University. The ages of all subjects ranged from 22 to 49 years old, with an average age of (30.8 ± 5.1) years old. The samples were divided into high E2 value group (>5 000 pmol/L, 78 cases) and low E2 value group ( 14, 68 cases) and low AFC value group (<7, 34 cases). Serum SERS analysis was established and Raman spectra of each group were detected. Orthogonal partial least squares discriminant analysis (OPLS-DA), receiver operating characteristic (ROC) curve and permutation test were used to analyze the signals. Results: The Raman spectrum morphology of serum samples was similar between high and low E2 value groups, high and low AMH value groups, and high and low AFC value groups, but the spectral peak intensity of the three indicators was different between the high and low value groups. In the OPLS-DA model, there was an obvious clustering trend in E2, AMH and AFC between the high and low value groups, and the areas under ROC curve were 0.996 and 0.996, 0.995 and 0.995, and 1 and 1 in high and low E2 value groups, high and low AMH value groups, and high and low AFC value groups, respectively. Conclusion: SERS has a potential to be used in the primary screening of female fertility. Serum SERS profle as an auxiliary method for early diagnosis of infertility is worthy of further study.

14.
Article in Chinese | WPRIM | ID: wpr-802045

ABSTRACT

Objective:To characterize and compare the chemical information of four extracts of Qingre Chushi (QRCS) decoction by liquid chromatography-mass spectrometry (LC-MS), and combine the chemical information of the four extracts with their results of anti-inflammatory effect for a multivariate statistical analysis, in order to identify the compounds directly relating to the anti-inflammatory effects of QRCS decoction. Method:Four extracts of QRCS decoction were characterized by UPLC-Q-TOF-MS:①ethanol extract+water extract,② ethanol extract+supernatant after water extraction and alcohol precipitation, ③ ethanol extract+precipitation after water extraction and alcohol precipitation,and ④ standard decoction. On the basis of the results of inhibition of the four above extracts on xylene-induced ear swelling in mice,multivariate statistical analysis[principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA)] were carried out to lock the chromatographic peaks with significant differences between group ① (the best pharmacological action group) and group ④ (standard decoction group). According to the accuracy of quasi-molecular ion and fragment ion data,and the reference materials and literature data,those chromatographic peaks were identified. Result:PCA could cluster the four extracts of QRCS decoction,and the differences between groups was reflected in the distance between groups. Group ④ (standard decoction) had the most significant differences with the other three groups, especially in the first principal component; group ① (ethanol extract+water extract),group ② (ethanol extract+supernatant after water extraction and ethanol precipitation) and group ③ (ethanol extract+precipitation after water extraction and ethanol precipitation) had certain differences in the second principal component. OPLS-DA was used to compare group ① (the best pharmacological action group) and group ④ (standard decoction group). Eleven chromatographic peaks with great contribution and high reliability to group differences,were identified as gentiopicrin,skimmin,baicalin,baicalin isomer,wogonoside,5,6,7-trihydroxy-8-methoxyflavone-7-O-glucurodonaldehyde,5,6-dihydroxy-6,8,2',3'-tetramethoxyflavone,salicin-6-C-arabinose-8-C-glucoside,plantamajoside and glycyrrhizic acid. Conclusion:In the mode of pectrum-effect combination, this study explores and identifies compounds relating to the anti-inflammatory effect of QRCS decoction,so as to provide the basis for screening the extraction and purification process and optimizing the formulation of preparation of Qingre Chushi decoction.

15.
Journal of Practical Radiology ; (12): 947-950,965, 2018.
Article in Chinese | WPRIM | ID: wpr-696945

ABSTRACT

Objective To characterize the biomarkers of urine samples for early diagnosis of colorectal cancer(CRC)using proton nuclear magnetic resonance (1H-NMR)combined with pattern recognition.Methods 400 MHz 1H-NMR was used to test the urine samples obtained from 23 patients with Ⅰ/Ⅱ stage CRC,40 healthy controls (HC)and 18 patients with esophageal cancer (EC). Pattern recognition through orthogonal partial least squares-discriminant analysis (OPLS-DA)was applied on 1H-NMR data to find urine metabolic differences between CRC and HC.Results OPLS-DA could effectively determine HC,patients withⅠ/Ⅱstage CRC and patients with esophageal cancer.Compared with HC,early stage CRC had significant decreases of choline,isocitric acid,lactamine,phenylalan, cysteine,creatinine,aspartic acid,hippurate acid,methylamine,dimethyl sulfone,and increases of acetoacetate,glutamine,glycocyamine,cis-aconitate, trans-aconitate,homocycteine in the urine samples.Conclusion Urine metabonomics based on NMRIndicates that glucose metabolism,amino acid metabolism,choline metabolism,energy metabolism and intestinal microflora are disturbance in colorectal cancer patients,which provide valuable metabolic information on the molecular level for early diagnosis of colorectal cancer.

16.
Article in Chinese | WPRIM | ID: wpr-687315

ABSTRACT

The present study is to establish the fingerprints for the quality evaluation of Ilicis Pubescentis Radix by HPLC-UV. The chromatographic conditions were defined as Phenomenex Luna C₁₈(4.6 mm × 250 mm, 5 μm). Mobile phase was acetonitrile-0.05% phosphoric acid in gradient elution, and the flow rate was 0.8 mL·min⁻¹.Column temperature was 30 °C and the injection volume was 10 μL.The detection wavelength was 210 nm. According to the similarity evaluation, the chemometric method was used to assess the quality of Ilicis Pubescentis Radix. The fingerprints of 16 batches of Ilicis Pubescentis Radix were established. There were 29 common peaks in the fingerprints and 12 common peaks were identified by reference substances. Fingerprints similarity of samples were greater than 0.92. The samples were classified into three groups by hierarchical cluster analysis combined with principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA), and seven components were the main markers that cause differences in the different batches of samples. By comparing the on-line UV spectra of chromatographic peaks, the chromatographic fingerprint was divided into three regions: region A showed seventeen main peaks (mainly lignans and phenolic acids); region B showed eight main peaks, which were proved as saponins; region C showed four main peaks, which were proved as other components. The established HPLC-UV fingerprint is highly specific, and can be used to evaluate the quality consistency of different batches of Ilicis Pubescentis Radix.

17.
Article in Chinese | WPRIM | ID: wpr-275121

ABSTRACT

In order to reveal the properties of polar metabolome in inflammatory cells, we selected LPS-induced RAW264.7 inflammatory cell models as the carrier for the research of metabolic fingerprint analysis. In this study, an ultra performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF/MS)-based metabolomics protocol was optimized for the extraction of polar metabolites from RAW264.7 cell line. Then orthogonal partial least squares discriminant analysis (OPLS-DA) was used to process the metabolic data, and finally, a total of 17 metabolites were selected and identified. The results showed that MeOH-CHCl3-H2O (8∶1∶1) was chosen as the optimal extraction solvent to achieve higher number of chromatographic peaks, with the best relative extraction efficiency and stability. Comparing with the normal cells, the inflammatory cells presented an abnormal metabolism in protein, carbohydrate, nucleotide and phospholipids. In this study, a UPLC-Q-TOF/MS-based metabolomics protocol for the polar metabolites from RAW264.7 cell line was developed, which may provide important information for the study of mechanism of inflammation and the anti-inflammatory drugs.

18.
Article in Chinese | WPRIM | ID: wpr-515108

ABSTRACT

AIM To establish the UPLC fingerprints of Bushen Qiangshen Tablets (Epimedii Folium,Cuscutae Semen,Rosae Laevigatae Fructus,etc.).METHODS The analysis of 50% ethanol extract of this drug was performed on a 40 ℃ thermostatic Agilent SB-C18 column (100 mm ×4.6 mm,2.7 μm),with the mobile phase comprising of acetonitrile-0.1% phosphoric acid flowing at 0.5 mL/min in a gradient elution manner,and the detection wavelength was set at 215 nm.Then the fringerprints were evaluated by cluster analysis,principal components analysis and orthogonal partial least squares discriminant analysis.RESULTS There were twenty common peaks in the UPLC fingerprints of twelve batches of samples,nine of which (protocatechuic acid,salidroside,chlorogenic acid,hyperin,specnuezhenide,epimedin C,icariin,kaempferide and baohuoside Ⅰ) were identified,with the similarities of 0.843-0.970.Twelve batches of samples could be divided into three types,and four differential markers,including specnuezhenide and chlorogenic acid,were found out.CONCLUSION This simple and reliable method can be used for the quality control of Bushen Qiangshen Tablets.

19.
Article in Chinese | WPRIM | ID: wpr-854043

ABSTRACT

Objective: To establish a method to fast identify the chemical constituents in the fruits of Schisandra sphenanthera and Schisandra chinensis by ultra performance liquid chromatography tandem with time-of-fight mass spectrometry with MSE data-acquistion mode (UFLC-Q-TOF-MSE) and provide the basis for high throughput characterization and distinction of the two two samples of Schisandra Michx by analyzing the remarkably different chemical components in the fruits between S. sphenanthera and S. chinensis. Methods: To rapidly identify the main chemical constituents in the fruits between S. sphenanthera and S. chinensis by using time-dependent scan mode, and combine with orthogonal partial least squares discriminant analysis (OPLS-DA) method to acquire significantly different constituents in the two samples of Schisandra Michx. Results: A total of 33 compounds were identified including 27 dibenzocyclooctene lignans. The differences of chemical compounds between the two sample groups could be obviously observed through the method of OPLS-DA in positive mode. There were 15 chemical ingredients of lignanes with significant differences identified in the two sample groups by comparison with retention time and mass spectra. Conclusion: The present study provides the basis for rapidly qualitative analysis of constituents and quantity control of the fruits in S. sphenanthera and S. chinensis.

20.
Clinics ; 67(4): 363-373, 2012. ilus, tab
Article in English | LILACS | ID: lil-623116

ABSTRACT

OBJECTIVES: Immunoglobulin A nephropathy is the most common cause of chronic renal failure among primary glomerulonephritis patients. The ability to diagnose immunoglobulin A nephropathy remains poor. However, renal biopsy is an inconvenient, invasive, and painful examination, and no reliable biomarkers have been developed for use in routine patient evaluations. The aims of the present study were to identify immunoglobulin A nephropathy patients, to identify useful biomarkers of immunoglobulin A nephropathy and to establish a human immunoglobulin A nephropathy metabolic profile. METHODS: Serum samples were collected from immunoglobulin A nephropathy patients who were not using immunosuppressants. A pilot study was undertaken to determine disease-specific metabolite biomarker profiles in three groups: healthy controls (N = 23), low-risk patients in whom immunoglobulin A nephropathy was confirmed as grades I-II by renal biopsy (N = 23), and high-risk patients with nephropathies of grades IV-V (N = 12). Serum samples were analyzed using proton nuclear magnetic resonance spectroscopy and by applying multivariate pattern recognition analysis for disease classification. RESULTS: Compared with the healthy controls, both the low-risk and high-risk patients had higher levels of phenylalanine, myo-Inositol, lactate, L6 lipids ( = CH-CH2-CH = O), L5 lipids (-CH2-C = O), and L3 lipids (-CH2-CH2-C = O) as well as lower levels of β -glucose, α-glucose, valine, tyrosine, phosphocholine, lysine, isoleucine, glycerolphosphocholine, glycine, glutamine, glutamate, alanine, acetate, 3-hydroxybutyrate, and 1-methylhistidine. CONCLUSIONS: These metabolites investigated in this study may serve as potential biomarkers of immunoglobulin A nephropathy. Point scoring of pattern recognition analysis was able to distinguish immunoglobulin A nephropathy patients from healthy controls. However, there were no obvious differences between the low-risk and high-risk groups in our research. These results offer new, sensitive and specific, noninvasive approaches that may be of great benefit to immunoglobulin A nephropathy patients by enabling earlier diagnosis.


Subject(s)
Adolescent , Adult , Female , Humans , Young Adult , Glomerulonephritis, IGA/diagnosis , Magnetic Resonance Spectroscopy/methods , Metabolomics/methods , Biopsy , Biomarkers/analysis , Case-Control Studies , Discriminant Analysis , Glomerulonephritis, IGA/metabolism , Glomerulonephritis, IGA/pathology , Kidney/pathology , Least-Squares Analysis , Protons , Sensitivity and Specificity
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