1.Determination of icariin and adenosine in Cordyceps Vigorine Tablet by HPLC
Qiang MA ; Yuxin ZHOU ; Haimin LEI ; Changhai WANG
Chinese Traditional Patent Medicine 2005;27(6):648-650
AIM: To establish HPLC for the determination of icariin and adenosine in Cordyceps Vigorine Tablet. METHODS:MetaChem Polaris ODS C18-A column(4.6 mm × 250 mm, 5 μm) was adopted; acetonitrile-water was the mobile phase; detection wavelength was set at 272 nm for icariin and at 260 nm for adenosine; column linearity within the range of 0. 374-2. 246 μg for icariin and 0. 348-1. 392 μg for adenosine, respectively. The average recovery and RSD were found to be (99.4 ± 1.84) % for icariin ( n = 6), (99.63 ± 1.29 ) % for adenosine,respectively. CONCLUSION: The method is convenient, fast, reliable to operate and suitable for the quality control of Cordyceps Vigorine Tablet.
2.Determination of tanshinone Ⅱ A in Compound Dangguifukang Capsule by RP-HPLC
Xinchun WANG ; Zhigeng YU ; Weijun CHEN ; Zhilin HU
Chinese Traditional Patent Medicine 2005;27(4):424-426
AIM: To establish a HPLC method for the determination of tanshinone Ⅱ A in Compound Danguifukang Capsule. METHODS: Analytic column: Reliasil C18(5μm, 250mm×4.6mm), protective column: (5μm, 12.50mm×4.6mm); mobile phase: methnaol-ultrapure water (80: 20); detective wavelength was at 270a good linearity within the range of 1×10-2-0.16μg, r=0.9995. The average recovery was 99.73% and RSD was 2.91%. CONCLUSION: The method is feasible, and simple to operate and suitable for the quality control of Compound Dangguifukang Capsule.
3.Comparative analysis of ursolic acid in Hawthorn leaves by HPLC
Ronghua LIU ; Boyang YU ; Shengxiang QIU ; Dan ZHENG
Chinese Traditional Patent Medicine 2005;27(3):318-322
AIM: To develop a simple HPLC for the determination of ursolic acid in Hawthorn leaves, and to compare ursolic acid content in Hawthorn leaves of different species, locations and growth stages, so as to supply some evidences for the exploitation and utilization of Hawthorn leaves reasonably. METHODS: By high-performance liquid chromatography method. Lichrospher C18 column (250 ×4.6 mm I. D. 5 μm); mobile phase, acetonitrile-water-orthophosphoric acid (85: 14.95: 0.05) with a flow-rate of 1.00 ml/min; column temperature at 30 ℃; injection volume, 5μl; UV detector at 210 nm. RESULTS: The detection limit (S/N=3) was less than 4. 024 μg/ml and the limit of quantification( S/N =10) was less than 12.05 μg/ml. The calibration curve showed good linear regression(r =0. 9999) within measurement ranges( 16.09 - 1030 μg/ml). The intra-day and interday variation were 0.71% and 6. 15%, respectively. The recoveries at low to high concentration were 89%-105%. Under these conditions, the ursolic acid content in different Hawthorn leaves were determined: 1.90%-1.95% in C. scabrifolia (Franch.) Rehd, 1.00%-1.45% in C. cuneata Sieb. & Zucc, 0.45%-0.65% in C.pinnatifida Bge. var. major N. E. Br.; In differnet growth stages of C. pinnatifida Bge. var. major N. E. Br. , the young leaves contain higher content of ursolic acid. CONCLUSION: The method is successfully applied to quantify ursolic acid in Hawthorn leaves. And the ursolic acid contents in Hawthorn leaves of differnent species are very different; C. scabrifolia (Franch.) Rehd contains the highest ursolic acid content in them. However, there is a little difference among different locations and growth stages for same species.
4.Preparation of fisetin solid dispersions
lai Chun FENG ; yang Yang DING ; jing Wen LI ; yin Jian YU ; ming Xi XU
Chinese Traditional Patent Medicine 2017;39(12):2503-2507
AIM To prepare fisetin solid dispersions.METHODS Melting method and solvent method were used for the preparation of solid dispersions,respectively.With carrier type,drug-carrier ratio and stirring time as influencing factors,accumulative dissolution rate as an evaluation index,the preparation was optimized by orthogonal test on the basis of single factor experiment.The interaction between drug and carrier was investigated by Fourier transform infrared spectroscopy (FTIR),and the drug existing state was analyzed by differential scanning calorimetry (DSC).RESULTS Solvent method was more suitable for the preparation of solid dispersions.The optimal conditions were determined to be PVPK-30 as a carrier,1 ∶ 12 for drug-carrier ratio,and 30 min for stirring time,the accumulative dissolution rate reached 90.87% within 20 min.There might be a hydrogen bond association between PVPK-30 and fisetin previously existing in amorphous or molecular state.CONCLUSION The dissolution rate of fisetin can be obviously increased after being prepared into solid dispersions.
5.Preparation of capsaicin phospholipid complex gel and its pharmacokinetic behaviors
jin Zi XU ; jian Zhang YANG ; Hui CHEN ; jun Ying YE
Chinese Traditional Patent Medicine 2017;39(12):2497-2502
AIM To prepare capsaicin phospholipid complex gel and to investigate its pharmacokinetic behaviors.METHODS Phospholipid complex was prepared by solvent evaporation method,whose PBS solution was then poured into Carbopol 940 solution to prepare gel.With feed ratio (phospholipid-capsaicin),capsaicin concentration and reaction time as influencing factors,phospholipid complex's recombination rate as an evaluation index,the preparation was optimized by central composite design-response surface method on the basis of single factor experiment.Rabbits were percutaneously administered with phospholipid complex gel and ordinary gel,respectively,after which LC-MS/MS was adopted in the content determination of capsaicin in plasma.Then the drug concentration-time curves for two gels were drawn,followed by the calculation of their pharmacokinetic parameters.RESULTS The optimal conditions were determined to be 2.3:1 for feed ratio,16 mg/mL for capsaicin concentration,2 h for reaction time,and 55 ℃ for reaction temperature,the recombination rate was 97.84%.The phospholipid complex gel demonstrated its superiority to the ordinary gel with higher Cmax,AUC0→∞,and lower tmax.CONCLUSION Capsaicin prepared into phospholipid complex gel has obviously increased bioavailability and improved percutaneous absorption.
6.Sequential therapy combined with ovulation induction of PCOS in endometrium of infertile women
li Xing TONG ; Yong TAN ; yun Yan YIN ; Ge ZHOU
Chinese Traditional Patent Medicine 2017;39(12):2491-2496
AIM To observe the endometrium receptivity of polycystic ovary syndrome patients and research advance of expression of HOXA10 in endometrium.METHODS Eighty PCOS patients were divided into treatment group and control group,40 persons in each group randomly.The control group was treated with clomiphene (CC) + human menopausal gonadotropin (HMG) + human chorionic gonadotropin (HCG),and the treatment group was treated with CC + HMG + HCG + Yin-Nourishing Yang-Supplementing.After 3 periods,take a record for below:endometrial thickness (Em) in the middle,advanced stage and mid-secretory phase of hyperplasia endometrii,the levels of spiral artery PI/RI in midluteum endometrium,the levels in serum of E2 and P in midluteum endometrium,the expression of HOXA10 mRNA from both groups,clinical pregnancy rate and abortion rate for each group.RESULTS Compared with the control group,endometrial thickness in the treatment group was increased and there is statistical difference in the middle and late follicle phases (P < 0.05),but there was no statistical difference in midluteum endometrium (P > 0.05);the level of E2 and P in the treatment group were raised (P <0.05) with statistical significance;PI and RI were obviously contracted (P < 0.01).Expression of HOXA10 mRNA was increased (P < 0.01).Compared with the control group,the treatment group had a significant difference in pregnancy rate (P < 0.05).The abortion rate was lower,but there was no statistical significance (P > 0.05).CONCLUSION Yin-Nourishing Yang-Supplementing Treatment can obtain higher pregnancy rate and lower abortion rate of PCOS patients and the mechanism might be associated with raising the expression of HOXA10 mRNA and reducing spiral artery PI/RI,also improving the function of corpus luteum treatment,then to improve the receptivity of endometrium.Yin-Nourishing Yang-Supplementing Treatment is well worth popularizing in further clinical application.
7.Preparation of colon-targeted pellets of Prunellae Spica effective components and the in vitro drug-release behaviors
wei Jian ZHANG ; Li LIU ; Qin WANG ; sheng De XU
Chinese Traditional Patent Medicine 2017;39(11):2273-2278
AIM To prepare colon-targeted pellets of Prunellae Spica effective components and to evaluate the in vitro drug-release behaviors.METHODS Fluidized bed coating method was adopted in the preparation of pellets.With in vitro accumulative release rate as an evaluation index,hydroxypropyl methyl cellulose (HMPC),polyacrylic resin (Eudragit S100) and triethyl citrate (TEC) amounts as influencing factors,orthogonal test was applied to optimizing the formulation.The in vitro drug-release behaviors were evaluated with rosmarinic acid content as an index.RESULTS The optimal formulation was determined to be 5% for HPMC amount,70% for Eudragit S100 amount,and 20% for TEC amount.The obtained pellets attained an accumulative release rate of more than 90% in pH 7.6 PBS (transportation for 2 h),while no drug dissolution was found in pH 1.0 HCl (transportation for 2 h) or pH 6.8 PBS (transportation for 3 h).CONCLUSION Colon-targeted pellets of Prunellae Spica effective components can achieve in vitro colon-targeted effect.
8.Evaluation of saponins in Paris Polyphylla var.chinensis from twenty-one growing areas
zhu Tie CHEN ; yan Fei WEN ; Tao ZHANG ; xia Yu YANG ; mao Qing FANG ; Hao ZHANG ; Dan XUE
Chinese Traditional Patent Medicine 2017;39(11):2345-2350
AIM To evaluate saponins in Paris Polyphylla Smith var.chinensis (Franch.) Hara from twentyone growing areas.METHODS HPLC was adopted in the content determination of pennogenins { pennogenin-3-O-β-D-glu (1→3) [α-L-rha (1→2)]-β-D-glu (PGGR),polyphyllinsⅥ,Ⅶ,H} and dioscins (gracillin,polyphyllins Ⅰ,Ⅱ,Ⅴ),then SPSS 22.0 software was used for principal component analysis and cluster analysis.RESULTS Pennogenin was the main kind of Paris Polyphylla var.chinensis saponins,and PGGR,polyphyllins Ⅰ,Ⅴ,Ⅶ,H were the main effective constituents of this medicinal material.The comprehension scores of seven growing areas were more than zero,which was in sequence of Bazhong > Qingchuan > Yanjin > Tongjiang > Nanchuan > Chongzhou > Hongya.Twenty-one batches of samples were divided into four types,which was similar to cluster analysis results.CONCLUSION Bazhong,Qingchuan,Chongzhou,Hongya,Tongjiang in Sichuan,Yanjin in Yunnan,and Nanchuan in Chongqing are suitable for cultivating Paris Polyphylla var.chinensis,which can guarantee the stability of saponins.
9.Chemical constituents from Metaplexis japonica
Peng HU ; lin Mao WANG ; Yue LI ; wei Jian CHEN ; Xiang LI
Chinese Traditional Patent Medicine 2017;39(11):2316-2318
AIM To study the chemical constituents from Metaplexis japonica (Thunb.) Makino.METHODS The dichloromethane fraction of 95% ethanol extract from M.japonica was isolated and purified by silica and preparative HPLC column,then the structures of obtained compounds were identified by physicochemical properties and spectral data.RESULTS Nine compounds were isolated and identified as dibutyl phthalate (1),(Z)-2-ethylidene-3-methylsuccinic acid (2),dehydrololiolide (3),medioresinol (4),isovanillin (5),vomifoliol (6),β-sitosterol (7),daucosterol (8),pregnenolone (9).CONCLUSION Compounds2-4 are isolated from genus Metaplexis for the first time,compounds 5-8 are first isolated from this plant.
10.Preparation of thermo-sensitive diammonium glycyrrhizinate binary liposome gel and the in vitro drug-release behaviors
Jing XUE ; Yuan GAO ; lei Xin WANG ; Fang LIU ; hua Bao HAO
Chinese Traditional Patent Medicine 2017;39(11):2284-2288
AIM To prepare thermo-sensitive diammonium glycyrrhizinate binary liposome gel and to evaluate the in vitro drug-release behaviors.METHODS Cold dissolution method was adopted in the preparation of gel.With gel transition temperature as an evaluation index,amounts of Poloxamer 407 (P407),Poloxamer 188 (P188) and polysaccharides from Bletillae Rhizoma as influencing factors,central composite design-response surface method was applied to optimizing the formulation.Then the in vitro drug-release behaviors were evaluated by HPLC and Franz vertical diffusion cell method.RESULTS The optimal formulation was determined to be 18% for P407 amount,4% for P188 amount,and 0.6% for polysaccharides' amount,the gel transition temperature was (37.5 ± 0.3) ℃.The accumulative release rate of obtained thermo-sensitive binary liposome gel was (65.52 ± 0.63) % within 48 h,which showed more obvious sustained-release effect as compared with liposome and thermosensitive gel.CONCLUSION Thermo-sensitive diammonium glycyrrhizinate binary liposome gel can reduce drug-release rate and increase its retention time in the rectum.