Comprehensive quality evaluation of Herba Clematidis Intricatae based on HPLC multi-index components, chemometrics combined with EW-TOPSIS method / 国际中医中药杂志

Objective:To comprehensively evaluate the quality of Herba Clematidis Intricatae through HPLC multi-index components, chemometrics combined with EW-TOPSIS. Methods:A total of 18 batches of Herba Clematidis Intricatae samples from seven provinces were collected. Contents of luteolin-7-O-glucoside, rutoside, hyperoside, quercitrin, quercetin, luteolin, apigenin and kaempferol in Herba Clematidis Intricatae were simultaneously determined by HPLC. Chemometrics method was used to comprehensively analyze the content determination results, and the main potential markers affecting the quality of Herba Clematidis Intricatae were analyzed. The quality of Herba Clematidis Intricatae from different origins was evaluated. Results:The eight components showed good linear relationships within their respective ranges ( r≥0.999 1), and accuracy was good ( RSD<2.0%). The chemometrics method showed that 18 batches of Herba Clematidis Intricatae could be clustered into 3 categories, showing certain regional differences. Rutoside, hyperoside and luteolin-7-O-glucoside were the indicative components affecting the difference of chemical constituents in Herba Clematidis Intricatae; results of EW-TOPSIS method showed that the optimum quality of Herba Clematidis Intricatae from Inner Mongolia and Liaoning, followed by those of Hebei, Shanxi and Shanxi, and lowest in Qinghai and Gansu. Conclusion:The established HPLC method is convenient and accurate, and combined with chemometrics and EW-TOPSIS method can be used for the comprehensive evaluation of the quality of Herba Clematidis Intricatae.

Quality evaluation and multi-spectral identification of origin herbs of Lonicerae Japonicae Flos based on grey correlation-TOPSIS method / 中国中药杂志

The grey correlation-TOPSIS method was used to evaluate the quality of the origin herbs of Lonicerae Japonicae Flos, and the Fourier transform near-infrared(NIR) and mid-infrared(MIR) spectroscopy was applied to establish the identification model of origin herbs of Lonicerae Japonicae Flos by combining chemometrics and spectral fusion strategies. The content of neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, secoxyloganin, isoquercitrin, isochlorogenic acid B, isochlorogenic acid A, and isochlorogenic acid C in six origin herbs of Lonicerae Japonicae Flos was determined by high-performance liquid chromatography(HPLC), and their quality was evaluated by the grey correlation-TOPSIS method. The Fourier transform NIR and MIR spectra of six origin herbs of Lonicerae Japonicae Flos(Lonicera japonica, L. macranthoides, L. hypoglauca, L. fulvotomentosa, L. confuse, and L. similis) were collected. At the same time, principal component analysis(PCA), support vector machine(SVM), and spectral data fusion technology were combined to determine the optimal identification method for the origin herbs of Lonicerae Japonicae Flos. There were differences in the quality of the origin herbs of Lonicerae Japonicae Flos. Specifically, there were significant differences between L. japonica and the other five origin herbs(P<0.01). The quality of L. similis was significantly different from that of L. fulvotomentosa, L. macranthoides, and L. hypoglauca(P=0.008, 0.027, 0.01), and there were also significant differences in the quality of L. hypoglauca and L. confuse(P=0.001). The PCA and SVM 2D models based on a single spectrum could not be used for the effective identification of the origin herbs of Lonicerae Japonicae Flos. The data fusion combined with the SVM model further improved the identification accuracy, and the identification accuracy of the mid-level data fusion reached 100%. Therefore, the grey correlation-TOPSIS method can be used to evaluate the quality of the origin herbs of Lonicerae Japonicae Flos. Based on the infrared spectral data fusion strategy and SVM chemometric model, it can accurately identify the origin herbs of Lonicerae Japonicae Flos, which can provide a new method for the origin identification of medicinal materials of Lonicerae Japonicae Flos.

Comprehensive quality evaluation of Tangwei capsule based on HPLC-QAMS multi-index quantitative determination combined with chemometrics and EW-TOPSIS method / 浙江大学学报·医学版

OBJECTIVES@#To detect the contents of Tangwei capsule main components with high performance liquid chromatography-quantitative analysis of multicomponents by single marker (HPLC-QAMS) method and to evaluate the quality with chemometrics and entropy weight-technique for order preference by similarity to an ideal solution (EW-TOPSIS).@*METHODS@#A symmetry C18 column and 0.1% formic acid-acetonitrile as mobile phase were used for HPLC of Tangwei capsule. The contents of 3'-hydroxypuerarin, puerarin, 3'-methoxypuerarin, methylnissolin-3-O-glucoside, calycosin, formononetin, rosmarinic acid, salvianolic acid B, dihydrotanshinone Ⅰ, cryptotanshinone, tanshinone Ⅰ, tanshinone ⅡA and cucurbitacin B in 15 batches of Tangwei capsule were determined simultaneously. The quality differences of 15 batches of samples were analyzed by chemometrics and EW-TOPSIS.@*RESULTS@#The HPLC-UV showed that 13 components had good linear relationships in corresponding concentration ranges (r≥0.9991). The relative standard deviations (RSD) of precision, repeatability and stability were all less than 2.00%. The average recovery rates were between 96.86% and 100.13%, and RSD were all less than 2.00%. Cluster analysis showed that 15 batches of samples were clustered into 3 groups. Partial least squares-discriminant analysis showed that salvianolic acid B, formononetin, puerarin, 3'-methoxypuerarin and rosmarinic acid were the main potential markers affecting the quality of Tangwei capsule. EW-TOPSIS analysis showed that the quality of S12-S15 was superior.@*CONCLUSIONS@#The analytical method established in this study can be used for the comprehensive evaluation of the quality of Tangwei capsule to provide laboratory support for its quality control and overall evaluation.

Quality Evaluation of Aurantii Fructus from Sichuan by Specific Chromatogram Combined with Chemometrics and Grey Correlation Analysis / 中国实验方剂学杂志

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.

Quality evaluation of Indigo Naturalis based on multi-component quantification combined with chemometrics / 中国药房

OBJECTIVE To evaluate the quality of Indigo Naturalis， and to provide reference for the quality control of Indigo Naturalis. METHODS UPLC-MS/MS method was used to determine the contents of 6 indole alkaloids （indigo， indirubin， isatin， tryptanthrin， indole and indole-3-carboxaldehyde） in Indigo Naturalis from different origins. Cluster analysis， principal component analysis and partial least squares-discriminant analysis （PLS-DA） were used to evaluate the quality of Indigo Naturalis from different origins. RESULTS The contents of indigo， indirubin， isatin， tryptanthrin， indole and indole-3-carboxaldehyde in Indigo Naturalis from different origins were 20 320.83-26 585.01， 1 327.69-3 102.25， 141.69-894.50， 2.17-5.27， 2.14-5.93 and 1.69-4.34 μg/g， respectively. The Indigo Naturalis from different areas were clustered into two categories by cluster analysis. Samples S1， S2， S4， S6， S7， S9 and S10 were clustered into category Ⅰ， and samples S3， S5， S8， S11 and S12 were clustered into category Ⅱ. Indigo Naturalis from different origins was evaluated with 3 principal components. The results showed that category Ⅰ sample scored higher and had better quality， while category Ⅱ sample scored lower and had worse quality. PLS-DA showed that indigo， indirubin， tryptanthrin and isatin were the main substances that reflected the quality difference of Indigo Naturalis. CONCLUSIONS The quality of Indigo Naturalis from different origins is different， and the quality of Indigo Naturalis of different batches from the same area is not stable. The quality evaluation method of Indigo Naturalis established in this paper is stable and reliable， which can provide a basis for the quality control of Indigo Naturalis.

Qualitative and quantitative evaluation of Flos Puerariae by using chemical fingerprint in combination with chemometrics method / 药物分析学报

In order to better control the quality of Flos Puerariae(FP),qualitative and quantitative analyses were initially performed by using chemical fingerprint and chemometrics methods in this study.First,the fingerprint of FP was developed by HPLC and the chemical markers were screened out by similarity analysis(SA),hierarchical clustering analysis(HCA),principal components analysis(PCA),and orthogonal partial least squares discriminant analysis(OPLS-DA).Next,the chemical constituents in FP were profiled and identified by HPLC coupled to Fourier transform ion cyclotron resonance mass spectrometry(HPLC-FT-ICR MS).Then,the characteristic constituents in FP were quantitatively analyzed by HPLC.As a result,31 common peaks were assigned in the fingerprint and 6 of them were considered as qualitative markers.A total of 35 chemical constituents were detected by HPLC-FT-ICR MS and 16 of them were unambiguously identified by comparing retention time,UV absorption wavelength,accurate mass,and MS/MS data with those of reference standards.Subsequently,the contents of glycitin,genistin,tectoridin,glycitein,genistein,and tectorigenin in 13 batches of FP were detected,ranging from 0.4438 to 11.06 mg/g,0.955 to 1.726 mg/g,9.81 to 57.22 mg/g,3.349 to 41.60 mg/g,0.3576 to 0.989 mg/g,and 2.126 to 9.99 mg/g,respectively.In conclusion,fingerprint analysis in combination with chemometrics methods could discover chemical markers for improving the quality control standard of FP.It is expected that the strategy applied in this study will be valuable for further quality control of other traditional Chinese medicines.

Identification of Growth Years of Scutellariae Radix By Characteristic Spectrum of Inorganic Elements Combined with Chemometrics / 中国实验方剂学杂志

ObjectiveTo obtain content characteristics of inorganic elements in Scutellariae Radix （aged 1-4 years）， and to explore the feasibility of identifying the growth years of Scutellariae Radix based on characteristic spectrum of inorganic elements combined with chemometric models. MethodAfter microwave digestion， the contents of Mn， Zn， Ca， Fe， Mg， Na， K， Cr， Cu， Se， As， Cd， Hg， Pb and Ni in 21 batches of Scutellariae Radix were determined by inductively coupled plasma atomic emission spectrometry （ICP-OES） and inductively coupled plasma mass spectrometry （ICP-MS）. Meanwhile， characteristic spectrum of inorganic elements in samples was drawn. The identification model was constructed to discriminate the growth years of Scutellariae Radix based on the combination of principal component analysis （PCA）， Fisher discriminant function and support vector machine （SVM）. ResultThe contents of Mn （7.79-36.48 μg·g-1）， Zn （10.12-31.43 μg·g-1）， Cu （6.38-17.20 μg·g-1）， K （2.98-13.89 μg·g-1）， Mg （3.45-7.78 μg·g-1） and Ca （2.32-7.09 μg·g-1） in Scutellariae Radix were detected by ICP-OES and ICP-MS， and their contents increased with the prolongation of growth years. PCA results showed that Cu， Ni， Cd， Na， Mg， Fe， Ca， Zn， Mn and Hg were characteristic elements of Scutellariae Radix. Samples with different years could be divided into four categories in the spatial characteristic diagram of Fisher discriminant analysis. The correct rate of SVM model for identifying the growth years of samples was 95.2%. ConclusionThis established method is accurate and rapid for discriminating the growth years of Scutellariae Radix， which can provide reference for the identification of other Chinese medicinal materials. It is suggested that some elements should be considered as indexes in subsequent construction of the quality evaluation system of Scutellariae Radix.

Comparative Analysis of Lonicera japonica Flower from Different Harvesting Periods Based on UV Fingerprint and Chemometrics / 中国实验方剂学杂志

ObjectiveTo investigate the quality variation of Lonicera japonica flower from different harvesting periods by ultraviolet visible（UV-Vis） fingerprint combined with chemometrics. MethodTwenty-five L. japonica flower samples from five harvesting periods， including young bud stage，green bud stage，white bud stage，silver and golden flower stages， were collected， with five samples for each stage. UV-Vis fingerprints of L. japonica flower from different harvesting periods were established in the context of the optimum extraction method based on the single factor experiment. The results showed that the absorption values at 209，216，226，250，280，303，318， and 350 nm were significantly different. Moreover，after data pretreatment and normalization，multivariate statistical analyses， such as principal component analysis （PCA），partial least squares discriminant analysis （PLS-DA），and orthogonal PLS-DA （OPLS-DA）were performed by SIMCA-P+ to establish the quality variation model of L. japonicas flower from harvesting periods. ResultAs revealed by PCA and PLS-DA， L. japonicas flower samples from five harvesting periods were clustered separately and closely in a harvesting time-dependent manner， suggesting that the content of components contained in samples from different harvesting periods was highly distinct and correlated with harvesting periods. The pairwise comparison of OPLS-DA indicated that triterpenoids or volatile oils were the main components causing the changes from the young bud stage to the green bud stage，and the content of them decreased. The main components from the green bud stage to the white bud stage were triterpenoids （or iridoids），volatile oils，phenolic acids， or flavonoids，and the content of them decreased， which was consistent with the HPLC result of chlorogenic acid. From the white bud stage to the silver flower stage， the main components were iridoids （increasing in content） and triterpenoids （or volatile oils） （decreasing in content）. The main altered components from the silver flower stage to the golden flower stage were triterpenoids （or volatile oils） whose content increased. ConclusionThis method is simple and feasible， which can provide references for the quality control of Chinese medicine.

Analysis of Chemical Constituents in Different Parts of Gentiana straminea Based on UPLC-Q-TOF-MS/MS / 中国实验方剂学杂志

ObjectiveUltra-performance liquid chromatography-quadrupole-time-of-flight tandem mass spectrometry （UPLC-Q-TOF-MS/MS） was used to analyze the chemical constituents in the aerial part and roots of Gentiana straminea from different areas of Qinghai province， and the main chromatographic peaks and differential components of different parts were identified. MethodThe chromatographic separation was performed on a Waters ACQUITY UPLC HSS T3 column （2.1 mm×100 mm， 1.8 μm） with 0.1% formic acid aqueous solution （A）-acetonitrile （B） as the mobile phase for gradient elution （0-1 min， 1%-13%B； 1-5 min， 13%-18%B； 5-7 min， 18%-50%B； 7-9.5 min， 50%-60%B； 9.5-11 min， 60%-99%B； 11-14 min； 99%B； 14-15 min， 99%-1%B； 15-16 min， 1%B）， the column temperature at 40 ℃， and the flow rate of 0.3 mL·min-1. Electrospray ionization （ESI） and negative ion full scan mode were selected for the mass spectrometric conditions to analyze the samples， and the detection range was m/z 50-1 200. Chemical constituents of the aerial part were qualitatively analyzed with the reference substances， literature information and ChemSpider. Principal component analysis （PCA） and orthogonal partial least squares discriminant analysis （OPLS-DA） were used to analyze the classification trend， correlation and differential chemical components between aerial part and roots of G. straminea. ResultA total of 68 components， including 24 iridoids， 13 flavonoids， 8 triterpenoids， 6 xanthones， 5 fatty acids， 4 saccharides， 3 phenolic glycosides， 2 alkaloids， 2 sterols and 1 lignan， were preliminarily identified from the aerial part of G. straminea. Among them， 42 components were firstly reported in 4 Gentiana species included in the 2020 edition of Chinese Pharmacopoeia. Eight differential components were screened out， namely sucrose， maltotriose， loganic acid， shanzhiside methyl ester， 6′-O-β-D-glucosylgentiopicroside， swertiamarin， gentiopicrin and isovitexin. ConclusionThe aerial part of G. straminea is rich in chemical constituents and has good medicinal potential. There were significant differences in the chemical components between the aerial part and roots of G. straminea， and the main differential components were iridoids， which could provide a basis for exploring efficacy differences in different parts of G. straminea.

Quantitative NMR spectroscopy and its application in quality control of Chinese medicinal injection / 中国中药杂志

Chinese medicinal injection, made of active components extracted from Chinese medicine or Chinese medicinal compound, is a novel dosage form of Chinese patent medicine in China and is pivotal in the traditional Chinese medicine(TCM) industry. The quality control standard of Chinese medicinal injection determines its safety and efficacy. The quantitative nuclear magnetic resonance(qNMR) spectroscopy is a non-targeted, non-invasive, and non-destructive technique with high reproducibility, short measurement time, convenient sample preparation, a broad range of linearity, and no requirement on the reference substance of tested components, which is advantageous as compared with traditional chromatographic methods, and it can provide information about the molecular composition of the tested samples. Therefore, in light of multiple challenges in the quality control of Chinese medicinal injection, such as complex composition, difficulties in quantitative analysis, and the shortage of reference substances, the application of qNMR spectroscopy combined with chemometrics techniques was proposed for the quality evaluation of Chinese medicine reference substances, Chinese medicinal injection, and intermediates in the production process, as well as for the stability analysis of Chinese medicinal injection. This study is expected to provide references for the application of qNMR spectroscopy in the quality control of Chinese medicinal injection.

Research progress and prospects for the use of plant metabolomics in quality evaluation of traditional Chinese medicinal materials / 药学学报

The quality of traditional Chinese medicine has a direct impact on the effectiveness and safety of its use, and is the premise necessary to ensure the healthy development of the traditional Chinese medicine industry. Comprehensive and accurate control and evaluation of the quality of medicinal materials is of great significance to the traditional Chinese medicine industry, but the complexity and dynamics of the chemical composition of medicinal materials makes their quality evaluation a challenge. Plant metabolomics provides an integrated and comprehensive analysis that is consistent with the holistic approach of traditional Chinese medicine. Chemical information therein promotes the establishment of a traceable system and provides new ideas and methods for the quality evaluation of medicinal materials. Plant metabolomics in the quality evaluation of medicinal materials is gradually increasing, and the core is the screening and identification of differential metabolites or specific marker compounds by means of stoichiometry. This study focused on the main factors that affect the quality of medicinal materials, such as origin, environmental adversity, varieties, harvest time, commercial specification and TCM processing. We describe the research progress in plant metabolomics combined with chemometrics analysis for the quality control and evaluation of medicinal materials, summarize existing problems, identify trends, and propose future research directions. Metabolomics plays an increasingly important role in the quality evaluation of medicinal materials, but the absolute qualitative and quantitative information of metabolomics needs to be further developed, and a single 'omics' technique is not sufficient for an in-depth analysis of medicinal value. In the future, standardization of plant metabolomics methods and a more complete database should be actively promoted, and plant metabolomics should be integrated into quality marker exploration. Plant metabolomics will need to be integrated with other 'omics' methods to improve the quality and evaluation system of medicinal materials.

GC-IMS Analysis of Volatile Components in Rhododendri Mollis Flos at Different Flowering Stages / 中国实验方剂学杂志

Objective:The volatile components of Rhododendri Mollis Flos were determined and the differences of volatile components at different flowering stages were compared and analyzed. Method:Gas chromatography-ion mobility spectrometry （GC-IMS） was used to detect the volatile components in Rhododendri Mollis Flos at different flowering stages （bud stage， initial flowering stage， half-flowering stage， blooming stage and late blooming stage）. GC-IMS spectra combined with cluster analysis， principal component analysis （PCA） and orthogonal partial least squares-discriminant analysis （OPLS-DA） were used to compare the differences and similarities of volatile components in different flowering stages. Result:A total of 70 volatile components in Rhododendri Mollis Flos at different flowering stages were detected， among which 67 were common components， and 47 were identified qualitatively， mainly alcohols， esters and aldehydes. Carveol was a special component at the late blooming stage. The content of alpha-terpineol is the highest at the initial flowering stage， but not at the blooming stage and late blooming stage. The relative contents of the active ingredients ［6-methyl-5-hepten-2-one， nonanal， alpha-terpineol， 1，8-cineole， linalool oxide， 1-octen-3-ol， （<italic>E</italic>）-3-hexenol］ showed a decreasing trend during flowering stages. GC-IMS spectra showed that the samples at different flowering stages had their own characteristic peak regions， and also had common regions. The results of cluster analysis， PCA and OPLS-DA all showed that the samples at different flowering stages were distinguishable. OPLS-DA was used to screen 19 different components to distinguish different flowering stages， including <italic>γ</italic>-butyrolactone， 1，8-cineole， ethyl hexanoate， etc. Conclusion:Rhododendri Mollis Flos samples at different flowering stages can be distinguished obviously， and the active substances in the volatile components are gradually dissipated with the degree of flower opening， which can provide reference for the improvement of material basis and the study of different flowering stages of Rhododendri Mollis Flos.

Comparison of Murraya exotica and Murraya paniculata by fingerprint analysis coupled with chemometrics and network pharmacology methods / 中国天然药物

There are two source plants for the traditional Chinese medicine Murrayae Folium et Cacumen (MFC) in Chinese Pharmacopoeia, i.e. Murraya exotica L. and M. paniculata (L.) Jack. Herein, a chemical comparison of M. exotica and M. paniculata by high performance liquid chromatography (HPLC) fingerprint analysis coupled with chemometrics and network pharmacology was performed. The main peaks in the fingerprints were identified by liquid chromatography coupled with ion trap/time-of-flight mass spectrometry (LC-IT-TOF-MS) and authenticated by references. The chemometrics results showed that the HPLC fingerprints of these two species were clearly divided into two categories using hierarchical cluster analysis (HCA) and principal component analysis (PCA), and a total of 13 significantly differentiated markers were screened out by orthogonal partial least squares-discriminant analysis (OPLS-DA). However, the following network pharmacology analysis showed that these discriminated markers were found to act via many common targets and metabolic pathways, indicating the possibly similar pharmacological effects and mechanisms for M. exotica and M. paniculata. The above results provide valuable evidence for the equivalent use of these two plants in clinical settings. Moreover, the chromatographic fingerprint analysis coupled with chemometrics and network pharmacology supplies an efficient approach for the comparative analysis of multi-source TCMs like MFC.

Quality evaluation of Aralia taibaiensis based on spectrum-activity relationship / 中国中药杂志

A spectrum-activity relationship is established with high performance liquid chromatography(HPLC) fingerprints and the in vitro antioxidant activity to improve the quality evaluation system of Aralia taibaiensis. The HPLC profiles of 12 batches of samples were collected, and the similarity evaluation, heat map analysis and principal component analysis were conducted for the chemometric study of the fingerprint data. Combined with grey correlation analysis, the contributions of the common peaks in the fingerprints to the antioxidant activity were clarified, and the important peaks reflecting the efficacy were identified. The results showed that 17 common peaks were found in 12 batches of A. taibaiensis samples, and 6 of them were identified as saponins. Similarity evaluation, heat map analysis and principal component analysis roughly classified the A. taibaiensis herbs into two categories, i.e.,(1) S1-S10, S12 and(2) S11. Twelve batches of samples showed different antioxidant activities in a dose-dependent manner. In particular, S9 had the strongest antioxidant activity, while S11 was the weakest in antioxidant capacity, which was basically consistent with the overall score results. The results of grey correlation analysis demonstrated that the 17 common peaks scavenged DPPH radicals in the following order: X_3>X_(17)>X_4>X_8>X_7>X_(13)>X_2>X_6>X_(11)>X_(10)>X_(16)>X_(12)>X_9>X_5>X_(14)>X_1>X_(15), and scavenged ABTS radicals in the order of X_4>X_3>X_7>X_8>X_2>X_(17)>X_(13)>X_6>X_(16)>X_(11)>X_5>X_(12)>X_(10)>X_9>X_(14)>X_1>X_(15). Among them, X_3, X_4, X_7(araloside C), X_8 and X_(17) were the important peaks reflecting the efficacy of A. taibaiensis, which were basically consistent with those contained in the principal component 1. In this study, the correlation between the HPLC fingerprints of 12 batches of A. taibaiensis and its antioxidant activity provides a reference for the Q-marker screening and quality control of A. taibaiensis.

Analysis of volatile oil components of different species of Curcumae Rhizoma based on GC-MS and chemometrics / 中国中药杂志

The volatile oil of Curcumae Rhizoma has many active components,which are the key to the quality of Curcumae Rhizoma. Exploring the difference between volatile oil of different kinds of Curcumae Rhizoma facilitates the quality control and rational application of resources. In this study,GC-MS was applied to realize online qualitative and semi-quantitative analysis of the chemical composition spectrum of volatile oil from Curcuma wenyujin( CW),C. phaeocaulis( CP),and C. kwangsiensis( CK). Forty components were identified and their fingerprints were compared and evaluated. Hierarchical cluster analysis( HCA),principal component analysis( PCA),and orthogonal partial least squares discrimination analysis( OPLS-DA) were adopted to analyze the overall and outlier data. The results showed that the whole data could be divided into three kinds according to each analysis mode,and the volatile components of Curcumae Rhizoma vary greatly among species. PCA explored the difference between outliers and the mean value of the group and found that some volatile oils from CW may be greatly affected by the origin. By OPLS-DA,the samples from Zhejiang were able to gather,but those from Guizhou remained isolated,indicating the influence of growing environment on Curcumae Rhizoma metabolites. Based on VIP results combined with the heat map,characteristic volatile oil components of Curcumae Rhizoma from different varieties were screened out: curdione and linalool for CW; 2-undecanone for CP; humulene,γ-selinene,and zederone for CK. The GCMS method established in this study describes Curcumae Rhizoma samples comprehensively and accurately,and the characteristic components screened based on chemometrics can be used to distinguish Curcumae Rhizoma from different varieties and give them unique pharmacodynamic significance,which is fast,convenient,stable,and reliable and supports the rational application of Curcu-mae Rhizoma resources. It is found that the region of origin has great influence on CW,which is worthy of further study.

Analysis on Feasibility of Electronic Nose Technology for Identification of Fritillariae Cirrhosae Bulbus from Authenticity and Specifications / 中国实验方剂学杂志

Objective:To establish a new fast and accurate method for identifying the authenticity and specifications of Fritillariae Cirrhosae Bulbus based on electronic nose technology， and to discuss the feasibility of this technology in the identification of decoction pieces. Method:Fritillariae Cirrhosae Bulbus was used as the research object， 80 batches of samples to be tested were collected， and the olfactory sensory data of the electronic nose were taken as independent variables （<italic>X</italic>）， the results of the method contained in the 2020 edition of <italic>Chinese Pharmacopoeia</italic> were taken as the focus， and the traditional empirical identification results were used as benchmarking information （<italic>Y</italic>）. Four chemometric methods， including discriminant analysis （DA）， least square support vector machine （LS-SVM）， principal component analysis-DA （PCA-DA） and partial least squares-DA （PLS-DA）， were used to establish the identification model ［<italic>Y</italic>=<italic>F</italic>（<italic>X</italic>）］ of authenticity and commodity specifications of Fritillariae Cirrhosae Bulbus， respectively. Wherein， the identification accuracy and time-consuming was taken as indicators to discuss the results. Result:After cross-verification by leave-one-out method， the correct rates of the above four models were 93.75%， 91.25%， 95.00% and 95.00%， respectively， and the PCA-DA and PLS-DA identification models were the best in terms of authenticity identification. In specification identification， the correct rates of these four models were 86.67%， 88.00%， 89.33% and 68.00%， respectively， and the PCA-DA identification model was the best. The electronic nose had a high accuracy in the identification of authenticity and specification model， and the time consuming was relatively short. Conclusion:Electronic nose technology can identify Fritillariae Cirrhosae Bulbus accurately and quickly， and has significant advantages in terms of timeliness and correct judgment rate.

Quality Evaluation of Citri Sarcodactylis Fructus from Different Origins Based on HPLC Fingerprint and Chemometrics / 中国实验方剂学杂志

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 C₁₈ 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.

FT-NIR associado a método quimiométrico para discriminar resíduos de antimicrobianos e antiparasitário no leite / FT-NIR coupled to chemometric method to discriminate antimicrobial and antiparasitic residues in milk

Introdução: O leite é um dos alimentos mais consumidos pelos seres humanos. Proteínas, vitaminas, gordura, carboidratos e sais minerais fazem parte de sua composição e desempenham importantes funções para a nutrição humana. A prática de adulteração no leite é antiga e ainda se faz presente nos dias de hoje em diversos países, inclusive no Brasil. A fim de obter lucro maior, alguns fornecedores costumam adicionar ao leite: água, amido, citrato, ureia, soda cáustica, cloreto de sódio, sacarose, soro do leite, melamina e outros componentes. No entanto, ainda há outro problema, o da contaminação do leite por medicamentos veterinários. Estes podem causar danos à saúde do consumidor e prejuízos para a produção de seus derivados. Objetivo: O presente trabalho propõe uma metodologia que permite detectar de maneira rápida a presença de resíduos de medicamentos veterinários em leites, dentro do limite máximo de resíduos de cada droga. Métodos: Fez-se o uso da espectroscopia no infravermelho próximo por transformada de Fourier associada à análise de componentes principais. A espectroscopia no infravermelho tem sido utilizada não somente para a autenticidade de laticínios, mas para determinar sua qualidade. Resultados: Conseguiu-se detectar resíduos de penicilina, oxitetraciclina e enrofloxacino, e também do antiparasitário ivermectina nas amostras de leites. Conclusão: A metodologia detectou de maneira rápida e precisa os resíduos das drogas analisadas, mesmo em concentrações muito baixas. Assim, é uma opção a outras existentes, já utilizadas para tal objetivo. (AU)

Introduction: Milk is one of the most consumed foods by humans. Proteins, vitamins, fat, carbohydrates and minerals are part of its composition and play important roles in human nutrition. The practice of adulteration in milk is old and is still present today in several countries, including Brazil. In order to obtain a higher profit, some suppliers usually add to the milk: water, starch, citrate, urea, caustic soda, sodium chloride, sucrose, whey, melamine and other components. However, there is still another problem, that of contamination of milk by veterinary medicines. These can cause damage to the health of the consumer and damage to the production of its derivatives. Objective: The present work proposes a methodology that allows to quickly detect the presence of residues of veterinary medicines in milk, within the maximum residue limit of each drug. Methods: The use of spectroscopy in the near infrared by Fourier transform associated with the analysis of principal components was used. Infrared spectroscopy has been used not only for the authenticity of dairy products, but to determine their quality. Results: It was possible to detect residues of penicillin, oxytetracycline and enrofloxacin, and also of the antiparasitic ivermectin in the milk samples. Conclusion: The methodology fastly and accurately detected the residues of the analyzed drugs, even in very low concentrations. Thus, it is an option to other existing ones, already used for this purpose. (AU)

Assessment of physicochemical, textural and microbiological properties of brazilian white mold surface-ripened cheeses: a technological approach / Avaliação das propriedades físico-químicas, de textura e microbiológicas de queijos brasileiros maturados com mofo branco: uma abordagem tecnológica

ABSTRACT: There are no specific technical regulations regarding the identity and quality of white mold surface-ripened cheeses in Brazil. These cheeses are sold both whole (Camembert-type) and in wedges (Brie-type). The aim of the study was to evaluate the physical and chemical properties; technological parameters and microbiological safety of 20 whole cheeses (Camembert-type) and 16 cheese wedges (Brie-type) produced in Brazil. Samples showed a wide range in sodium (91.0-731.0 mg/100 g, cheeses wedges) and calcium (238.0-1100.0 mg/100g, whole cheeses) contents. The cheese groups presented no significant differences in relation to the majority of the analyzed parameters. Listeria monocytogenes was reported in 5% of the whole cheese samples. The other microbiological parameters were in accordance with the current legislation, RDC no 12/2001 of Anvisa. The comparative assessments between these two cheeses indicated that they are different. In addition, the wide range of results indicated a lack of processing standardization. The mean values of the physicochemical and textural parameters should be considered as recommended for these cheeses in Brazil.

RESUMO: No Brasil, não há uma regulamentação técnica específica sobre a identidade e qualidade de queijos maturados com mofo branco na superfície. Estes queijos são comercializados inteiros (tipo Camembert) e em cunhas (tipo Brie). O objetivo da pesquisa foi avaliar as propriedades físicas e químicas; parâmetros tecnológicos e marcadores microbiológicos de 20 queijos inteiros (tipo Camembert) e 16 cunhas de queijo (tipo Brie) produzidos no Brasil. Os teores de sódio e cálcio apresentaram elevada amplitude (8,0 e 4,6 vezes o valor mínimo, respectivamente). Os valores médios destes queijos não apresentaram diferenças significativas em relação à maioria dos parâmetros analisados. Listeria monocytogenes foi encontrada em 5% das amostras de queijo tipo Camembert. Os demais parâmetros microbiológicos estavam de acordo com a legislação vigente, RDC no 12/2001 da Anvisa. Esta avaliação comparativa entre estes dois queijos indica que são diferentes. Além disso, os valores com elevada amplitude correspondem a falta de padronização do processamento. Os valores médios poderiam ser considerados como recomendados para estes queijos no Brasil.

TGA/Chemometrics addressing innovative preparation strategies for functionalized carbon nanotubes / 药物分析学报

In this work, functionalized carbon nanotubes (CNTs) using two polyamine polymers, polyethyleneimine (PEI) and polyamidoamine dendrimer (PAMAM), were investigated by thermal analysis in order to address preparation strategies to obtain low cytotoxic compounds with the ability to conjugate micro-RNAs and, at the same time, to transfect efficiently endothelial cells. Thermogravimetric analysis (TGA) was coupled to chemometrics as a novel analytical strategy to characterize functionalized CNTs from different preparation conditions. In particular, two starting materials were considered:very small CNTs and carboxylated CNTs (CNT-COOH) in order to examine the affinity with polymers. Chemometrics permitted to compare results from TGA and to investigate the effect of a number of factors affecting the synthesis of coated nanotubes including a different amount of involved polymer and the time required for the suspension for a satisfactory and reproducible preparation procedure. The results demonstrated the effectiveness of TGA as a tool able to address synthesis of coated CNTs to be employed as efficient drug delivery vectors in biomedical applications.