OBJECTIVE:To establish a method for the contents determination of emodin,rhein,aloe-emodin,chrysophanol, physcion,geniposide,chlorogenic acid in Yinchenhao decoction and its dispensing granule,and to compare the difference among the above-mentioned ingredients. METHODS:HPLC was adopted to determine the contents of emodin, rhein, aloe-emodin, chrysophanol and physcion:the column was Ecosil C18 with mobile phase of acetonitrile-0.5% phosphoric acid(gradient elution)at a flow rate of 1 ml/min,the detection wavelength was 254 nm,column temperature was 35 ℃,and injection volume was 20 μl. When determining the content of geniposide by HPLC,the column was Ecosil C18 with mobile phase of acetonitrile-water(13∶87, V/V)at a flow rate of 1 ml/min,the detection wavelength was 238 nm,column temperature was 35 ℃,and injection volume was 20 μl. When determining the content of chlorogenic acid by HPLC,the column was Ecosil C18 with mobile phase of acetonitrile-0.5% phosphoric acid (10∶90,V/V) at a flow rate of 1 ml/min,the detection wavelength was 327 nm,column temperature was 35 ℃,and injection volume was 20 μl. RESULTS:The linear range was 2-20 μg/ml for emodin(r=0.996 5),5.2-52.0 μg/ml for rhein(r=0.998 5),2.6-26.0 μg/ml for aloe-emodin(r=0.999 9),1.0-10.4 μg/ml for chrysophanol(r=0.999 9),1.0-10.0 μg/ml for physcion(r=0.999 8),20-200 μg/ml for geniposide(r=0.999 9),20-200 μg/ml for chlorogenic acid(r=0.999 9);RSDs of precision,stability and reproducibility tests were lower than 3%;recoveries were 91.1%-96.9%(RSD=2.0%,n=6)for emodin、93.9%-96.1%(RSD=0.8%,n=6)for rhein、90.9%-93.4%(RSD=1.2%,n=6)for aloe-emodin、88.5%-92.7%(RSD=1.8%,n=6) for chrysophanol、82.1% -87.9%(RSD=2.5% ,n=6)for physcion,100.4% -102.0%(RSD=0.7% ,n=6)for geniposide、101.1%-102.2%(RSD=0.4%,n=6) for chlorogenic acid. CONCLUSIONS:The method is simple,stable and reproducible,and can be used for the simultaneous contents determination of active ingredients in Yinchenhao decoction and its dispensing granule. The contents of active ingredients in Yinchenhao dispensing granule are obviously higher than those in its decoction.

Objective:To study the extraction process of Zhengtian Capsules (Radix Paeoniae Alba, Ramulus Vncariae cum Vnics, Rhizoma Chuanxiong, Herba Ephedrae, Herba Asari, etc.). Methods: Uniform design was used in the experiments, the alcoholic extract rate of the total alkaloid of Ramulus Uncariae cum uncis which was determined by titrimetric methods to evaluate the factor levels; and the water extraction process was studied by orthogonal design with the content of paeoniflorin which was determined by HPLC and with the yield of extracta sicca as the detective markers. Results: The optimum alcohol extraction factors were 8 times of 90% ethanol, infusing up to 72 hours. The optimum process of water decoction was to add 14 times amount of water, decocting for 3 times (2h, 1h, 1h in turn). Conclusion: According to the optimum extracting factors, the active substance can be extracted sufficiently.

A novel system was developed for the rapid determination of vitexin, vitexin-2″-O-rhamnoside, rutin, and hyperoside in the extract of hawthorn(Crataegus pinnatifida Bge.) leaves with microemulsion liquid chromatography(MELC). The effect on the chromatography of varying the operating paramers was studied. The optimized MELC system with microemulsion was consisting of 1.0%(w/w) brij35-1.1%(w/w) n-butanol-0.1%(w/w) n-octanol-0.3%(v/v) triethylamine, the pH was adjusted to 2.5 with phosphoric acid. The type and concentration of surfactant, types of oil phase, the pH and triethylamine as the organic additive in microemulsion played an important role for separation of four flavonoids. MELC analysis was performed on a Venusil ASB C_(18) analytical column (150 mm× 4.6 mm, i.d., 5 μm). The flow rate was set at 0.8 mL/min and the eluent was detected at 340 nm for the four flavonoids. The calibration curves of the four flavonoids are linear(r>0.9995) over the concentration range of 0.95-140.0 mg/L. The mean recoveries are 98.6% to 101.6%. The results indicate that the optimized method was successfully applied to the analysis of four important flavonoids in the extract of hawthorn leaves.

Objective To optimize the formulation in preparation of dropping pills with total glucosides in Radix Paeoniae Alba and evaluate its accumulative release percentage in vitro.Methods With the hardness,roundness,and adhesion as the evaluation,orthogonal design was conducted.With dissolution rate of 12 h as the indices,according to the uniform design,the optimum coating formulation of Eudragit RL and RS was established.Results The dropping pills met the criterion of formulation,and the preparation release met the characteristics of the sustained release of the first order kinetics.Conclusion The optimal formulation is simple,which provides the basis for further development of new preparations of total glucosides in Radix Paeoniae Alba.

Objective To prepare generic irbesartan tablets and to evaluate its consistency of dissolution tests.Methods Using the original drugs (irbesartan) as reference drug,the single factor experiments were applied to investigating the type and amount of adhesive,tablet hardness,water content of tablets,and coating weight.ZRS-8G Dissolution Tester was used to conduct the dissolution tests which were carried on four different dissolution media.Then the similar factor (f2) was adopted to evaluate the similarity of dissolution between the original drug and generic drug.Results As the stabilizer,3％ HPMC-E5 was more stable than 5％ PVP K30.It had no difference of dissolution between original and generic drugs when the amount of adhesive,tablets hardness and water content were within the range of investigation.And the coating weight was 2％ to 3％.Moreover,the f2 values of original drug and generic drug were all greater than 50 in different dissolution media.Conclusion Thef2 results indicate a similarity in the dissolution behavior of reference drug and generic irbesartan tablets prepared by the single factor experiments.And the preparation process of generic irbesartan tablets is stable.

Objective To develop a formulation of generic Valsartan Tablets and evaluate the quality consistency in vitro.Methods Diovan(R)~ HCT (80 mg) was used as the reference drug.In order to determine the best formulation and the best preparation processing,the single factor experiments were applied to determining the best formulation and the best preparation processing.And dissolution test was used as the evaluation index in the single factor experiments.Meanwhile the dissolubility of generic Valsartan Tablets and original preparation was investigated in four different media to evaluate the similarity of dissolution by calculating similar factor (f2).Results The dissolution was above 85％ of three batches of generic Valsartan Tablets in the phosphate buffer (pH 6.8).The similar factors were all more than 50 in the water,hydrochloric acid solution (pH 1.2),and acetate buffer solution (pH 4.5).Conclusion The f2 similarity factor results indicate a similarity in the reference drug and generic Valsartan Tablets which were developed by single factor experiments,which means the quality of genetic Valsartan Tablets is qualified.

OBJECTIVETo investigate the fragmentation pathway of vitexin and isorhamnetin-3-O-beta-D-rutinoside with CID-TOF-MS.

METHODEquipped with an LC-MS was carried out using an ultra-performance liquid chromatography, electrospray ionization quadrupole collision-induced dissociation-TOF-MS.

RESULTESI-MS spectrum showed [M-H]- base peak of m/z 431. 0958 and m/z 623.1566. The CID-MS of vitexin showed five basic fragment ions, three of which corresponded to the glucosyl ring fracture: m/z 353, 341 and 311; other two were benzyl ion m/z 283, aglycone ion m/z 269. In addition, two low abundance ions, namely, m/z 161 and m/z 117, generated by RDA cracking ions, were also characteristic ions. The CID-MS of isorhamnetin-3-O-beta-D-rutinoside showed six main characteristic fragments ions corresponding to the loss of rhamnosyl m/z 477 and the glycosyl ring fracture: m/z 387, 357 and 311, and aglycone ion m/z 315. In addition, B ring generated m/z 300 and m/z 271 and C ring generated m/z 243 and the RDA cleavage generated m/z 151 and m/z 125.

CONCLUSIONThose fragment ions can be used to quickly identify vitexin and isorhamnetin-3-O-beta-D-rutinoside.

Apigenin ; chemistry ; Disaccharides ; chemistry ; Drugs, Chinese Herbal ; chemistry ; Flavonoids ; chemistry ; Molecular Structure ; Spectrometry, Mass, Electrospray Ionization ; instrumentation ; methods

Objective: To study the pharmacodynamic effect of Reganling Oral Liquid(RGL) in treating wind heat epidemic syndrome. Methods: After RGL was administered ig to experiment animals, we observed its antifebrile effect by using pathologic hectic rabbit caused by typhoid bacterin and pathologic hectic rat caused by injection of 2,4 dinitro phenol, anti inflammation effect by weighing the tampon acestoma in rat, anti anaphylaxis effect by using delay anaphylactoid mice caused by injection of 2,4 dinitrochloro benzene. The Liquid Tube Observing Method was used to investigate the bacteriostatic activity of RGL on eight kinds of germina in vitro . Results: RGL could evidently inhibit the raising of animal heat caused by bacterin and chemical, and also could markedly restrain the weight of tampon acestoma in rat and delay anaphylactoid in mice. RGL also had remarkably bacteriostatic activity on eight kinds of germina in vitro which mainly caused wind heat epidemic syndrome. Conclusion: RGL had the evident effects of antifebrile, anti inflammation, anti anaphylaxis and bacteriostatic activity in vitro .