3.Establishment of HPLC fingerprints of Cajanus cajan leaves and determination of two constituents
Aili XU ; Xiaoli BI ; Sumei LI ; Yangxue LI ; Jieyi JIANG ; Buming LIU
Chinese Traditional Patent Medicine 2017;39(7):1435-1439
AIM To establish the HPLC fingerprints of Cajanus cajan (L.) Millsp.leaves and to determine the contents of orientoside and luteolin.METHODS The analysis of 65% methanol extract from C.cajan leaves was performed on a 25 ℃ thermostatic Agilent Zorbax SB-C18 column (4.6 mm ×250 mm,5 μm),with the mobile phase comprising of methanol-1% acetic acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 260 nm.RESULTS There were twenty-one common peaks in ten batches of samples (S1-S10),whose similarities were more than 0.950,except for that of S3 (0.516).Orientoside and luteolin showed good linear relationships within the ranges of 0.089 5-3.960 μg and 0.015 5-0.408 μg,whose average recoveries were 99.43% (RSD =1.32%) and 98.50% (RSD =0.82%),respectively.The contents of two constituents in the samples from three growing areas (Guangdong,Yunnan and Hainan) showed obvious differences.CONCLUSION This simple,accurate and reproducible method can be used for the quality control of C.cajan leaves.
4.Phenols from Vitex negundo
Ting WEN ; Jie HUANG ; Xiaojun HUANG ; Chunlin FAN ; Ying WANG ; Wencai YE
Chinese Traditional Patent Medicine 2017;39(7):1431-1434
AIM To study the phenols from Vitex negundo Linn..METHODS The ethyl acetate fraction of 70% ethanol extract from V.negundo was isolated and purified by silica,Sephadex LH-20 and ODS column,then the structures of obtained compounds were identified by spectral data.RESULTS Seven compounds were isolated and identified as luteolin-4'-O-β-D-glucopyranoside (1),isoorientin 6-O-caffeate (2),3,4,5-tricaffeoyl quinic acid (3),(+)-pinoresinol-4-O-β-D-glucoside (4),methyl isoferuloyl-7-(3,4-dihydroxyphenyl) lactate (5),benzyl 7-O-β-D-glucoside (6) and oresbiusin A (7).CONCLUSION All the compounds are isolated from this plant for the first time,and compounds 1,3,5-7 are first isolated from genus Vitex.
5.Chemical constituents from twigs of Trigonostemon lutescens
Changshui YANG ; Suqiao HAN ; Xinyu SHEN ; Xing WANG ; Ping BU
Chinese Traditional Patent Medicine 2017;39(7):1427-1430
AIM To study the chemical constituents from twigs of Trigonostemon lutescens Y.T.Chang et J.Y.Liang.METHODS The ethyl acetate fraction of 95% ethanol extract from T.lutescens twigs was isolated and purified by silica,Sephadex LH-20 and MCI column,then the structures of obtained compounds were identified by physicochemical properties and spectral data.RESULTS Ten compounds were isolated and elucidated as 3-O-acetyloleanolic acid (1),methyl 3-acetoxy-12-enly-oleanen-28-oate (2),taraxerone (3),spiciflorin (4),simiarenol (5),β-sitosterol palmitate (6),3,3',4-tri-O-methylellagic acid (7),β-sitosterol (8),stigamasterol (9),palmitic acid (10).CONCLUSION Compounds 1-6 are isolated from genus Trigonostemon for the first time,compounds 7 and 9 are first obtained from this plant.
6.Chemical constituents from Sonchus oleraceus
Zhenzhen ZHAO ; Songsong ZHAO ; Bin GUO
Chinese Traditional Patent Medicine 2017;39(7):1423-1426
AIM To study the chemical constituents from Sonchus oleraceus L..METHODS The 50% ethanol fraction of 70% ethanol extract from S.oleraceus was isolated and purfieid by macroporous resin,Sephadex LH-20,ODS and RP-HPLC column,then the structures of obtained compounds were identified by physiochemical properties and spectral data.RESULTS Eleven compounds were isolated and identified as isololiolide (1),bluemenol A (2),5-methoxyisolariciresinol (3),lyoniresinol (4),syringaresinol mono-β-D-glucoside (5),robinin (6),loliolide (7),dehydrovomifoliol (8),5-(1 '-hydroxyethyl)-methyl nicotinate (9),2-methoxy-1,4-benzenediol (10),4-methoxyphenol (11).CONCLUSION Compounds 1-9 are isolated from genus Sonchus for the first time.
7.Chemical constituents from Vigna umbellate
Qiao CHEN ; Xiaoyue LIU ; Yanan SHI ; Jia CAO ; Tingting ZHANG ; Nan XU
Chinese Traditional Patent Medicine 2017;39(7):1419-1422
AIM To study the chemical constituents from Vigna umbellata Ohwi et Ohashi.METHODS The ethyl acetate fraction of 80% ethanol extract from V.umbellata was isolated and purified by silica,Sephadex LH-20 and ODS column,then the structures of obtained compounds were identified by spectral data and physicochemical properties.RESULTS Twelve compounds were isolated and elucidated as (+) catechin (1),(-) epicatechin (2),3-furanmethanol-β-D-glucopyranoside (3),myricetin-3-O-β-D-glucopyranoside (4),quercetin7-O-β-D-glucopyranoside (5),(+) catechin-3-O-β-D-glucopyranoside (6),(+) catechin-5-O-β-D-glucopyranoside (7),quercetin-3 '-O-α-L-rhamnoside (8),(±) dihydroquercetin (9),quercetin (10),ethyl gallate (11),propanediol (12).CONCLUSION All the compounds are isolated from V.umbellata for the first time,and compounds 4,8,9,11,12 are first obtained from genus Vigna.
8.Secondary metabolites from Aspergillus petrakii
Yuling HUANG ; Liying MA ; Xianguo RONG ; Deguo LI ; Desheng LIU ; Weizhong LIU
Chinese Traditional Patent Medicine 2017;39(7):1415-1419
AIM To study the secondary metabolites from Aspergillus petrakii.METHODS The ethyl acetate extract liquid of A.petrakii fermentation broth was isolated and purified by silica,ODS,Sephadex LH-20 and RP-HPLC column,then the structures of obtained compounds were identified by spectral data and physicochemical properties.RESULTS Thirteen compounds were isolated and identified as R-(-)-mellein (1),3-(1-hydroxyethyl)-7-hydroxy-l-isobenzofuranone (2),(-)-semivioxanthin (3),endocrocin (4),p-hydroxyphenylethanol (5),p-hydroxyphenylacetamide (6),hydroquinone (7),adenosine (8),cyclo (Phe-Val) (9),cyclo (Phe-Ile) (10),cyclo (Tyr-Ala) (11),cyclo (Leu-Ile) (12),cyclo (Leu-Leu) (13).CONCLUSION All the compounds are isolated from A.petrakii for the first time.
9.Quality standard for Ershiwuwei Feibing Pills
Xiang LI ; Yali LIU ; Pei QIAO ; Jing ZHANG ; Zhiqing LIU ; Qin HUANG ; Jing CHEN ; Chunfeng ZHAN
Chinese Traditional Patent Medicine 2017;39(7):1410-1414
AIM To establish the quality standard for Tibeten medicine Ershiwuwei Feibing Pills [Inula racemosa Hook.f.,Swertia bimaculata (Sieb.et Zucc.) Hook.Thors.ex Clarke,Phyllanthus emblica Linn.,Terminalia billerica (Gaertn.) Roxb.,etc.].METHODS TLC was applied to the qualitative identification of L racemosa,S.bimaculata,P.emblica and T.billerica,and HPLC was adopted in the quantitative determination of alantolactone,oleanolic acid,gallic acid and hydroxysafflor yellow A.RESULTS The TLC spots were clear without negative interference.Alantolactone,oleanolic acid,gallic acid and hydroxysafflor yellow A showed good linear relationships within the ranges of 4.324-216.2 μg/mL (r =0.999 9),32.222-1 611.1 μg/mL (r =0.999 9),4.072-203.6 μg/mL (r =0.999 9) and 4.266-213.3 μg/mL (r =0.999 9),whose average recoveries (RSDs) were 100.6% (0.93%),100.3% (2.1%),101.5% (3.0%) and 100.1% (1.8%),respectively.CONCLUSION This simple method can be used for the rapid quality control of Ershiwuwei Feibing Pills.
10.Simultaneous determination of eight constituents in Erchen Mixture by HPLC
Chinese Traditional Patent Medicine 2017;39(7):1406-1409
AIM To develop an HPLC method for the simultaneous content determination of narirutin,hesperidin,nobiletin,3,5,6,7,8,3',4'-heptemthoxyflavone,tangeratin,dehydrotumulosic acid,dehydropachymic acid and pachymic acid in Erchen Mixture (Citri reticulatae Pericarpium,Poria,Pinelliae Rhizoma,etc.).METHODS The analysis of methanol extract of this drug was performed on a 35 ℃ thermostatic Agilent TC-C18 column (4.6 mm × 250 mm,5 μm),with the mobile phase comprising of acetonitrile-0.1% formic acid flowing at 0.9 mL/min in a gradient elution manner.RESULTS Eight constituents showed good linear relationships within their own ranges (r > 0.999 0),whose average recoveries were 96.94%-99.69% with the RSDs of 0.88%-1.76%.CONCLUSION This accurate,reliable and reproducible method can be used for the quality control of Erchen Mixture.