1.Determination of formononetin and calycosin from Zhengqifuzheng Preparation by HPLC
Fangdi HU ; Shilan FENG ; Jianxiong ZHAO
Chinese Traditional Patent Medicine 1992;0(09):-
AIM: To establish a method of RP-HPLC for determination of calycosin and formononetin in Zhengqifuzheng Preparation(Radix Astragali, Fructus Ligustri Lucidi, etc.). METHODS: Kromasil ODS column(5?m,4.6mm?250mm) was used to determine two isoflavoniods with water-methanol gradient elution, at column temperature of 25℃, flow-rate of 1.0mL?min -1 and detection wavelength at 254nm. RESULTS: The average recoveries of formononetin and calycosin in Zhengqifuzheng Capsules were 96.53% and 98.34% and RSD were 2.25% and 4.01%, respectively, the average recoveries of formonoenetin and calycosin in Zhengqifuzheng Granules were 97.20% and 95.65% and RSD were 2.66% and 2.32%, respectively. CONCLUSION: The method is sample, reliable, accurate, practical, and can provid a new idea to study the quality standard of this preparation.
2.Sulfated modification and anticoagulant activity in vitro of sulfated glucan isolated from the aqueous extract of Hedysarum polybotrys.
Long GUO ; Yinglai YANG ; Tao YANG ; Ziheng LIU ; Shilan FENG
Acta Pharmaceutica Sinica 2013;48(11):1665-70
SHG was sulfated by chlorosulfonic acid-pyridine method, and six samples which we got were prepared in different reaction conditions. There is a characteristic absorption peak near 260 nm in UV spectra and there are two characteristic absorption peaks near 1240 cm(-1) and 810 cm(-1) in the FT-IR. Degree of sulfation (DS) was calculated by elemental analysis and turbidimetry. Under the same conditions the absorption peaks become strong with the DS increase. The anticoagulant activity of SHG and sulfated modification samples was evaluated by the classic coagulant assays of prothrombin time (PT), activated partial thrombin time (APTT) live enzymes, and plasma thrombin time (TT). Results show that sulfated SHG has a good anticoagulant activity in vitro, and DS increased activity within a certain range.
3.Determination of jasminoidin and paeoniflorin in Chizhihuang Capsules by HPLC
Hao TANG ; Shilan FENG ; Guangtao MIN ; Xiang GAO ;
Chinese Traditional Patent Medicine 1992;0(05):-
AIM: To establish a HPLC quality control for Chizhihuang Capsules(Radix Paeoniae Rubra, Fructus Gardeniae, Radix et Rhizoma Rhei, etc.). METHODS: Shim pack C 18 column was used, and jasminoidin and paeoniflorin were determined at the same time and detection wavelength at 230nm. RESULTS: The standard curve of jasminoidin was linear in the range of 0.30~1.50?g. The average recovery and RSD were 99.58 and 1.57% ( n =5), respectively. The standard curve of paeoniflorin was linear in the range of 0.26~ 1.30?g . The average recovery and RSD were 99.11 and 1.29% ( n =5), respectively. CONCLUSIONS: This method is a convenient, reliable and accurate for the quality control of Chizhihuang Capsules.
4.Chromatography fingerprint of Baitiao Radix Codonopsis in Gansu Province by HPLC
Shilan FENG ; Fangdi HU ; Xin LIU ; Jianxiong ZHAO
Chinese Traditional Patent Medicine 1992;0(07):-
AIM To establish chromatography fingerprint of Radix Codonopsis. METHODS HPLC was applyed on a Hypersil ODS column with water-methanol gradient elution, flow-rate of 0.8 ml?min -1 . Determination of content of atractylenodie Ⅲ adopted ELSD and PAD with methanol-water(67∶ 33), flow-rate of 1.0 ml?min -1 , column temperature at 30?C , ELSD:carried-gas flow-rate of 2.2 L?min -1 , drift-tuber temperature was 80?C ;PAD:wavelength was 220 nm. RESULTS 25 common peaks were picked up, their similarity among 10 batchs of samples was more than 98.12 % based on marker composition(Atractylenolide Ⅲ). CONCLUSION The chromatography fingerprint of Baitiao Radix Codonopsis could be used as their characteristic chromatography fingerprint of hydrophobic fraction.
5.Coumarins from Peucedanum harry-smithii var. subglabrum.
Wen LI ; Shilan FENG ; Fangdi HU ; Erlin CHEN
China Journal of Chinese Materia Medica 2009;34(10):1231-1234
The root of Peucedanum harry-smithii var. subglabrum was extracted with methanol, then separated with solvents at different polarity into four fractions: aqueous (H2O), ethyl acetate (AcOEt), chloroform (CHCl3) and petroleum ether (DAB-6). From AcOEt psoralen, bargapten, xanthotoxin, marmesin, umbelliferone, scopoletin, (+/-) peuformosin, Pd-I b, (+/-) selinidin, praeruptorin D were isolated by column chromatography on silica gel, using petroleum ether/ethyl acetate as eluent. The structures of the coumarins were identified by 1H-NMR and 13C-NMR.
Apiaceae
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chemistry
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Coumarins
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chemistry
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isolation & purification
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Magnetic Resonance Spectroscopy
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methods
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Plant Roots
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chemistry
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Umbelliferones
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chemistry
6.Qualitative and Quantitative Analysis of Bushen Jiannao Grains by Ultra Performance Convergence Chromatography
Ruijuan ZHU ; Bo WANG ; Fang HU ; Can LI ; Xiaoya LIU ; Shilan FENG ; Wei ZHOU
Chinese Journal of Analytical Chemistry 2015;(2):288-293
An ultra performance convergence chromatographic ( UPC2 ) method was established for the attribution analysis of the main peaks as well as the quantitative determination of echinacoside andβ-ecdyserone in Bushen Jiannao Grains. The samples were extracted with ethanol and separated on Waters ACQUITY UPC2TM BEH column (100 mm × 3. 00 mm, 1. 7 μm), with a gradient supercritical CO2-0. 05%phosphoric acid-methanol solvent system at 40 ℃. The flow rate was 0. 8 mL/min, the detection wavelength was set at 248 nm and the injection volume was 1 μL. Results showed that all the main peaks in the fingerprint were clearly attributed. The peak named 12 wasβ-ecdyserone with the content of 380μg/g and the peak named 15 was echinacoside with the content of 9. 562 mg/g. The method was simple, eco-friendly, accurate and reliable compared with HPLC and UPLC.
7.Evaluation preparation technology of Xiaochaihu granules using fingerprint-peak pattern matching
Yuqiong WU ; Yuqiang GOU ; Jing HAN ; Yingyan BI ; Shilan FENG ; Fangdi HU ; Chunming WANG
Journal of Pharmaceutical Analysis 2011;01(2):119-124
An approach was proposed to evaluate preparation technology by means of fingerprint-peak matching technology of high performance liquid chromatography with diode array detector (HPLC-DAD).Similarity and hierarchical clustering analysis (HCA) were applied to identify the 15 batches of Xiaochaihu granules from different manufacturers and our laboratory,and peak pattern matching between the composite formulae and Radix Bupleuri Chinensis,which was one of the main ingredients of Xiaochaihu granules,was utilized to evaluate the preparation technology of Xiaochaihu granules via the indexes of the relative deviation of retention time (RT) and UV spectrum feature similarity of their corresponding peaks.Eleven matching peaks were found between Xiaochalhu granules and Radix Bupleuri Chinensis.However,the saikosaponin A and saikosaponin D,which are the important active components in Radix Bupleuri Chinensis,were not found in Xiaochaihu granules from any manufacturers.The peak areas of 11 characteristic peaks of Xiaochaihu granules samples formed a matrix of 11 × 15.The result of HCA showed that Xiaochaihu granules samples were divided into four kinds of category.Xiaochaihu granules samples from the same manufacturer were basically clustered of the same category.The results suggested that the saikosaponin A and saikosaponin D are prone to structural transformation under the condition of decoction and in the presence of the organic acidic components.These active components,existing in raw herb,might transform to a series of non-active secondary saikosaponin due to unfavourable preparation technology.So the conventional decoction-based preparation technology of Xiaochaihu granules might greatly affect its quality and therapeutic effectiveness. This study demonstrates that fingerprint-peak matching technology can not only be used for quality control of this composite formulae,but also provide some guidance for preparation technology of Xiaochaihu granules.
8.Quantification of six bioactive compounds in Zhenqi Fuzheng preparation by high-performance liquid chromatography coupled with diode array detector and evaporative light scattering detector
Yikai SHI ; Fang CUI ; Fangdi HU ; Yingyan BI ; Yufeng MA ; Shilan FENG
Journal of Pharmaceutical Analysis 2011;01(1):20-25
A simple and accurate high-performance liquid chromatography (HPLC) coupled with diode array detector (DAD) and evaporative light scattering detector (ELSD) was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation (ZFP).The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis (HCA),which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.
9.Determination of polysaccaride content in Radix Hedysari by HPLC
Bing LI ; Shilan FENG ; Xiaohua LIU ; Dan MA ; Xiaodong LI ; Fangdi HU ; Yipei ZHANG
Chinese Traditional Patent Medicine 1992;0(05):-
AIM: To establish a method for determing polysaccaride content of Radix Hedysari(Hedysarum Polybotrys Hand-Mazz). METHODS: To determine content of Radix Hedysari polysaccaride by HPLC and ELSD. RESULTS: The composes of Radix Hedysari polysaccaride Ⅰ、Ⅱ、Ⅲ、Ⅳ are all Rhamnose、Arabinose、Xylose、Glucose、Galactose,the average content of polysaccharides is 25.34%、24.23%、15.08%、17.24%. CONCLUSION: The contents of Radix Hedysari polysaccaride in Radix Hedysari can be determined by HPLC.
10.Quantification of six bioactive compounds in Zhenqi Fuzheng preparation by high-performance liquid chromatography coupled with diode array detector and evaporative light scattering detector
Yikai SHI ; Fang CUI ; Fangdi HU ; Yingyan BI ; Yufeng MA ; Shilan FENG
Journal of Pharmaceutical Analysis 2011;01(1):20-25
A simple and accurate high-performance liquid chromatography(HPLC)coupled with diode array detector(DAD)and evaporative light scattering detector(ELSD)was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation(ZFP).The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis(HCA),which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.