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Objective: To establish a UPLC fingerprint method and a method for the content determination of 3,5-O-dicaffeoylquinic acid of Aucklandiae Radix, and provide a comprehensive evaluation of the drug from different habitats. Methods: UPLC analysis was performed on a YMC Trait C18 (100 mm × 2.1 mm, 1.9 μm), with a mobile phase consisting of acetonitrile-0.05% phosphoric acid at the flow rate of 0.30 mL/min. The fingerprint detection wavelength was 254 nm and the content determination detection wavelength of 3,5-O-dicaffeoylquinic acid was 327 nm, meanwhile, the column temperature was controlled at 30 ℃. Similarity analysis, hierarchical clustering analysis, and principal component analysis were undertaken to investigate the fingerprints of 13 batches of Aucklandiae Radix. Results: UPLC fingerprint of Aucklandiae Radix was established and eight common peaks were designated. The results showed that the quality of the batches of samples were not stable. Samples collected from the same region and different regions both had certain differences, as well as the content determination of 3,5-O-dicaffeoylquinic acid. Conclusion: The proposed method offered a fast, holistic, and effective method for the quality control of Aucklandiae Radix.
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Objective: To establish an HPLC method for fingerprint analysis of Xintongtai Granules (XG) for its quality control. Methods: The chromatographic behaviors were obtained by a Phenomenext Luna C18 column (250 mm × 4.6 mm, 5 μm) with gradient elution using 0.1% formic acid solution-methanol as the mobile phase. The detection wavelength was 280 nm, the volume flow rate was 1.0 mL/min, and the column temperature was 30 ℃. The samples of 10 batches of XG were determined, and the chromatographic fingerprint similarity evaluation system of Chinese medicine (2012 edition) was used to establish the common pattern of XG fingerprints, and the similarity was calculated. Then the common peaks were identified by the reference chromatogram. Results: HPLC fingerprints of XG were established by the determination of 10 batches of samples. The similarity was above 0.95. A total of 26 common peaks were calibrated. Three mutual peaks (No. 21, 22, 26 peaks) were from Salviae Miltiorrhizae Radix et Rhizoma, eight mutual peaks (No. 4—10, 16 peaks) were from Puerariae Lobatae Radix, seven mutual peaks (No. 13, 15, 17—20, 23 peaks) were from Aurantii Fructus, No. 12 peak was from Chuanxiong Rhizoma, No. 14 peaks was from Glycyrrhizae Radix et Rhizoma, No. 1 peak was shared by Notoginseng Radix et Rhizoma and Glycyrrhizae Radix et Rhizoma, No. 2 peaks was shared by Notoginseng Radix et Rhizoma, Aucklandiae Radix, and Crataegi Fructus, No. 3 peaks was shared by Chuanxiong Rhizoma and Aucklandiae Radix, No. 11 peaks was shared by Puerariae Lobatae Radix and Curcumae Radix, the No. 24 peaks was shared by Chuanxiong Rhizoma and Aurantii Fructus, and No. 25 peaks was shared by Curcumae Radix and Aurantii Fructus. The common peaks were all assigned to each medicinal material and identified by reference chromatograms: No. 7, 12, 22, and 26 peaks were puerarin, ferulic acid, salvianolic acid B, and tanshinone IIA. Conclusion: The similarity results of 10 batches of samples indicate that the particle preparation process is stable and feasible, and the established HPLC fingerprint method is stable and reliable. It can be used to measure the stability of XG production process and the controllability of finished product quality.
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Objective: To establish an odor fingerprint with electronic nose technology to qualitatively identify Aucklandiae Radix odor from different producing areas. Methods: Eight batches of Aucklandiae Radix samples from eight different producing areas were collected. The odor information of each sample was obtained by electronic nose. The LDA algorithm based on Fisher’s identification criterion and the nonlinear dimensionality reduction LLE + SMA algorithm were used to distinguish the Aucklandiae Radix odor of different origins. Results: It was found that the LDA algorithm based on Fisher’s discriminant criterion could not distinguish the Aucklandiae Radix scent of different producing areas. Some of the samples in the place of origin had a lot of overlap, and the LLE + SMA algorithm could distinguish the odor very well. It can completely distinguish eight batches of Aucklandiae Radix samples from eight different producing areas. Conclusion: It is feasible to apply the electronic nose technology to the odor differentiation of Aucklandiae Radix from different producing areas, and provide new ideas and methods for the quality evaluation of Aucklandiae Radix.
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Objective:To establish a supercritical fluid chromatography(SFC) method for separating and purifying costunolide and dehydrocostus lactone in Aucklandiae Radix. Method:With supercritical carbon dioxide as the mobile phase,the effect of six factors, such as type of chromatographic columns,modifiers and modifiers ratio, flow rate of mobile phase,pressure and temperature, on the separation process of supercritical fluid chromatography were explored. The target components were separated and prepared by semi-preparative supercritical fluid chromatography. High performance liquid chromatography and nuclear magnetic resonance were used to analyze the components and study the thermodynamic regularity of the chromatographic process. Result:C18 column (10 mm×250 mm,5 μm) was adopted, with supercritical fluid dioxide as the mobile phase,the ratio of methanol was 0.13%,the flow rate was 12 mL·min-1,column pressure was 13 MPa,column temperature was 318℃, and detection wavelength was 225 nm. The sample was injected for 20 times,crude extract was 4 mg,and each target component was collected according to the chromatogram. Its purity was determined to be more than 99%by HPLC,and its structure was determined as costunolide and dehydrocostus lactone by NMR. Under this condition,the SFC separation process was normal-phase chromatography. Conclusion:The method can be used to prepare effective components of Aucklandiae Radix with a high purity and low solvent residue.
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Objective To comprehensively evaluate the Aucklandiae Radix quality by combining gray correlation method and FCM (Fuzzy C-Means) algorithm. Methods HPLC method was used to determine the content of costunolide and dehydrocostus, and the content of volatile oil was determined by steam distillation. The gray correlation method was used to sort the quality of Chinese herbal medicines, and the FCM algorithm was used to classify the quality of medicines. Results The average correlation degree of Aucklandiae Radix from different producing areas was: Yunnan > Guangdong > Guangxi > Hunan> Sichuan > Bozhou > Beijing > Hebei. FCM algorithm divided samples into three categories: Yunnan, Guangdong and Guangxi were in the high quality group; Hunan and Sichuan were in the medium quality group; Beijing, Bozhou, and Hebei were in the low quality group. Conclusion Constructing an integrated pattern recognition model system for evaluating the quality of Chinese medicinal materials, and the fuzzy clustering algorithm was adopted for the first time in Aucklandiae Radix. The purpose of this study is to form a kind of research method of Aucklandiae Radix quality evaluation and provide a way to guide and apply the new methods of modern pattern recognition and data mining in the application of traditional Chinese medicine quality evaluation.
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OBJECTIVE:To improve the quality standard for Qiwei maqianzi pills.METHODS:TLC was used for the qualitative identification of Chebulae Fmctus and Aucklandiae Radix in the preparation.HPLC method was used for the content determination of hydroxy safflor yellow A,brucine and strychnine in preparation.The determination was performed on Phenomenex Prodigy C18 column with mobile phase consisted of methanol-acetonitrile-0.7％ phosphoric acid soulution(26 ∶ 2 ∶ 72,V/V/V,for hydroxy safflor yellow A),acetonitrile-0.01 mol/L sodium heptanesulfonate mixed with same quantity of 0.02 mol/L potassium dihydrogen phosphate (pH adjusted to 2.8 using 10％ phosphoric acid,21 ∶ 79,V/V,for brucine and strychnine) at the flow rate of 1.0 mL/min.The detection wavelengths were 403 nm (for hydroxy safflor yellow A) and 260 nm (for brucine and strychnine).The column temperature was 25 ℃C,and the injection volume was 10 μL.RESULTS:TLC spots of Chebulae Fructus and Aucklandiae Radix were clear and well-separated without interference from negative control.The linear range was 6.29-62.94 μg/mL for hydroxy safflor yellow A(r=0.999 3),1.83-18.30 μg/mL for brucine(r=0.999 4) and 2.11-21.11 μg/mL for strychnine (r=0.999 6).RSDs of precision,stability and reproducibility tests were lower than 2.0％.The recoveries were 101.66％-104.91％(RSD=1.14％,n=6),99.58％-104.55％ (RSD=1.75％,n=6) and 101.22％-104.04％ (RSD=0.99％,n=6),respectively.CONCLUSIONS:Improved standard can be better used for quality control of Qiwei maqianzi pills.
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Objective:To optimize the paper-roasted technology of Aucklandiae Radix. Methods:With methanol-water (65: 35) as the mobile phase, the contents of costunolide and dehydrocostuslactone were determined by HPLC. Senna was used to make diarrhea model in mice, and the sample decoction was administered for the mice by i. g at the dose of 10 g·kg-1 and the diarrhea index was de-termined. The paper-roasted technology of Aucklandiae Radix was optimized by L9 (34 ) orthogonal design taking the contents of cost-unolide and dehydrocostuslactone, and the diarrhea index in mice as the indices with the paper-roasted time, the paper-roasted temper-ature and the layer number as the influencing factors. Results:The variance analysis results show that the layer number and the paper-roasted temperature has the significant impact on the contents of costunolide and dehydrocostuslactone and the diarrhea index in mice. The best paper-roasted technology of Aucklandiae Radix was as follows:a layer of paper was covered by 4mm Aucklandiae Radix and repeated the same operation 5 times, and put them in drying baker at 120℃ for about 2 hours. After the essential oil of Aucklandi-ae Radix permeated on the paper with burnt flavor and dark brown in color, Aucklandiae Radix could be taken out. Conclusion:The optimum paper-roasted technology of Aucklandiae Radix is reasonable and feasible, which can provide reference for the establishment of the quality standard for paper-roasted Aucklandiae Radix pieces and the expanding of the clinical application.