Guizhi Fuling capsule (GFC), a traditional Chinese medicine (TCM) with effects of promoting blood circulation and dissipating blood stasis, has been widely used in the clinic. Because of the complex matrix and various chemical structure types, quality control of GFC remains great challenge. In the present study, an ultra performance liquid chromatography hybrid triple-quadrupole mass spectrometry (UPLC-QQQ MS) method with ultrafast positive/negative ionization switching was developed for simultaneous determination of 18 bioactive components in GFC, including methyl gallate, ethyl gallate, oxypaeoniflorin, benzoic acid, albiflorin, paeonolide, paeoniflorin, 1, 2, 3, 4, 6-pentagalloylglucose, mudanpioside C, benzoyloxypaeoniflorin, benzoylpaeoniflorin, pachymic acid, amygdalin, cinnamaldehyde, paeonol, cinnamic acid, 4-hydroxybenzoic acid, and gallic acid. Separation was performed on an Agilent Zorbax Extend-C18 column (2.1 mm × 50 mm, 1.8 μm), using a gradient elution with acetonitrile and water containing 0.1% formic acid. Cholic acid was selected as the internal standard. This newly developed method was fully validated for linearity, precision, accuracy, and stability, and then applied to quality assessment of GFC. Finally, the batch-to-batch reproducibility of GFC samples was evaluated by the cosine ration and Euclidean distance method, which showed high quality consistency. The results demonstrated that the developed method pro vided a reasonable and powerful manner for quality control of GFC.
Chemical Fractionation ; methods ; Cholic Acid ; standards ; Chromatography, High Pressure Liquid ; Chromatography, Liquid ; Drugs, Chinese Herbal ; analysis ; chemistry ; Quality Control ; Reference Standards ; Reproducibility of Results ; Tandem Mass Spectrometry

Brown algae are well known as a source of biologically active compounds, especially those having antioxidant activities, such as phlorotannins. In this study we examined the antioxidant activities of crude phlorotannins extracts (CPEs) obtained from Sargassum hemiphyllum (SH) and fractionated according to the molecular weights. When CPEs were administrated at a dose of 30 mg/kg to Kunming mice pre-treated with carbon tetrachloride (CCl4), the levels of oxidative stress indicators in the liver, kidney and brain were significantly reduced in vivo. All the components of various molecular weight fractions of CPEs exhibited greater scavenging capacities in clearing hydroxyl free radical and superoxide anion than the positive controls gallic acid, vitamin C and vitamin E. Particularly, the components greater than 30 kD obtained from ethyl acetate phase showed the highest antioxidant capacities. These results indicated that SH is a potential source for extracting phlorotannins, the algal antioxidant compounds.
Animals ; Antioxidants ; isolation & purification ; pharmacology ; Ascorbic Acid ; pharmacology ; Brain ; drug effects ; metabolism ; pathology ; Carbon Tetrachloride ; antagonists & inhibitors ; toxicity ; Carbon Tetrachloride Poisoning ; drug therapy ; metabolism ; pathology ; Chemical Fractionation ; methods ; Gallic Acid ; pharmacology ; Hydroxyl Radical ; antagonists & inhibitors ; metabolism ; Kidney ; drug effects ; metabolism ; pathology ; Liquid-Liquid Extraction ; methods ; Liver ; drug effects ; metabolism ; pathology ; Male ; Mice ; Mice, Inbred Strains ; Oxidation-Reduction ; Oxidative Stress ; drug effects ; Phaeophyta ; chemistry ; Sargassum ; chemistry ; Superoxides ; antagonists & inhibitors ; metabolism ; Tannins ; isolation & purification ; pharmacology ; Vitamin E ; pharmacology

The purpose of this study was to design and prepare a biocompatible microemulsion of Andrographis paniculata (BMAP) containing both fat-soluble and water-soluble constituents. We determined the contents of active constituents of BMAP and evaluated its bioavailability. The biocompatible microemulsion (BM), containing lecithin and bile salts, was optimized in the present study, showing a good physical stability. The mean droplet size was 19.12 nm, and the average polydispersity index (PDI) was 0.153. The contents of andrographolide and dehydroandrographolide in BMAP, as determined by high performance liquid chromatography (HPLC), were higher than that in ethanol extraction. The pharmacokinetic results of BMAP showed that the AUC0-7 and AUC0→∞ values of BMAP were 2.267 and 27.156 μg·mL(-1)·h(-1), respectively, and were about 1.41-fold and 6.30-fold greater than that of ethanol extraction, respectively. These results demonstrated that the bioavailability of and rographolide extracted by BMAP was significantly higher than that extracted by ethanol. In conclusion, the BMAP preparation displayed ann improved dose form for future clinical applications.
Andrographis ; chemistry ; Chemical Fractionation ; instrumentation ; methods ; Chromatography, High Pressure Liquid ; Diterpenes ; analysis ; isolation & purification ; Drugs, Chinese Herbal ; analysis ; isolation & purification ; Emulsions ; chemistry

This paper was aim to optimize the purification technology of Rehmanniae Radix Praeparata extract with macroporous adsorption resin. With the content of manninotriose as index, the absorptive flow and time were investigated, as well as kinds, amount, flow of eluent. D-101 type macroporous adsorption resin was the best choice for the purification of manninotriose. The optimized parameters were as follows: the content of manninotriose at 161.16-53.72 mg x g(-1), absorption time 240 min, eluting solvent of purified water, volume flow at 1.5 BV x h(-1), and eluant volume at 6 BV. D-101 type macroporous adsorption resin could significantly increase the purity of Rehmanniae Radix Praeparata extract with the advantage of high absorption, remove most part of impurity, and the effect of semi-works production was better.
Adsorption ; Chemical Fractionation ; Chromatography, Liquid ; instrumentation ; methods ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; Rehmannia ; chemistry ; Resins, Synthetic ; chemistry

The study was using the orthogonal test and making the extraction rates of icariin, ferulic acid, epimedin A, epimedin B, epimedin C, baohuoside I and ligustilide determinated by HPLC multiwavelength switch, gradient elution and multi-index comprehensive weighted scoring method (weight coefficient was 0.47: 0.16: 0.07: 0.07: 0.08: 0.06: 0.09) as evaluation index, combine with SPSS 16.0 software to optimizing the best extraction. It was Yinpian soak 1 h, 12 times more than the volumn of 50% ethanol solution, by heating reflux extraction for 60 min. The compliance test indicates that the optimized compatibility extraction technology is stable and practical, and it has provided an experimental basis for compound preparation technology research of Epimedium brevicornu and Ligusticum chuanxiong.
Chemical Fractionation ; methods ; Chemistry, Pharmaceutical ; methods ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; Epimedium ; chemistry ; Ligusticum ; chemistry

A method was established for the simultaneous analysis of 25 trace elements and heavy metals in polysccharides from Liuwei Dihuang prescription, including Li, Be, B, Ti, Mg, Al, V, Cr, Mn, Co, Fe, Ni, Cu, Zn, Ga, As, Sr, Cd, Sn, Sb, Ba, Hg, Tl, Pb, Bi. The different rate of elemental extraction in Al, Fe, Mg, B, Ti, Mn, Zn, Sr, Ba was made in water and different concentration of alcohol. The samples, digested via microwave, calibrated by internal standard elements such as Ge and In, with bush branches and leaves as the controlled reference standard, were inlet into ICP-MS to analyze the contents of the 24 trace elements and heavy metals. The detection limits of the 24 elements were in the range of 0.007-2.225 µg · L(-1), while the RSD was below ≤ 4. 0%, with their recovery ranging from 84. 1% to 116%. Big different of the elemental extraction rates could be found by using different ethanol solutions. The method is simple, rapid and accurate, and can be used for the quality control of trace elements and heavy metals in Liuwei Dihuang polysccharides. With the aid of the obtained result, we may increase the extraction of necessary element while making an attempt at multi-element speciation in polysccharides from Liuwei Dihuang.
Chemical Fractionation ; Drugs, Chinese Herbal ; chemistry ; Mass Spectrometry ; methods ; Polysaccharides ; chemistry ; isolation & purification ; Trace Elements ; chemistry ; isolation & purification

The extracting technology of salidroside, tyrosol, crenulatin and gallic acid from Rhodiolae Crenulatae Radix et Rhizoma was optimized. With extraction rate of salidroside, tyrosol, crenulatin and gallic acid as indexes, orthogonal test was used to evaluate effect of 4 factors on extracting technology, including concentration of solvent, the dosage of solvent, duration of extraction, and frequency of extraction. The results showed that, the best extracting technology was to extract in 70% alcohol with 8 times the weight of herbal medicine for 2 times, with 3 hours once. High extraction rate of salidroside, tyrosol, crenulatin and gallic acid were obtained with the present technology. The extracting technology was stable and feasible with high extraction rate of four compounds from Rhodiolae Crenulatae Radix et Rhizoma, it was suitable for industrial production.
Chemical Fractionation ; methods ; Chemistry, Pharmaceutical ; methods ; Coumarins ; isolation & purification ; Drugs, Chinese Herbal ; isolation & purification ; Gallic Acid ; isolation & purification ; Glucosides ; isolation & purification ; Phenols ; isolation & purification ; Phenylethyl Alcohol ; analogs & derivatives ; isolation & purification ; Rhizome ; chemistry ; Rhodiola ; chemistry

In order to established a method for simultaneous determination of isoquercitrin, astragaline, quercetin and kaempferol in Lysimachia clethroides, the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate ([HMIM]PF6) methanol was used as the ultrasound-assisted extraction solvent combing with RP-HPLC. A Purospher star RP-C1 column was used with the mobile phase of aceto- nitrile, methanol and 0. 4% phosphate acid by gradient elution at the detection wavelength of 360 nm. The flow rate was 0.7 mL x min(-1), and the column temperature was the room temperature. Under the optimized conditions, the linear ranges were 2.54 x 10(-2)-2. 54, 2.50 x 10(-2)- 2.50, 1.54 x 10(-3)-0.154, 1.49 x 10(-3)-0.149 microg for isoquercitrin, astragaline, quercetin and kaempferol, respectively. The average recoveries of the four constituents were 101.1%, 98.90%, 101.0%, 101.6%, respectively. The method was green, simple, rapid and accurate, and provided a valid method for analysis of isoquercitrin, astragaline, quercetin and kaempferol in L. clethroides.
Chemical Fractionation ; instrumentation ; methods ; Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal ; analysis ; isolation & purification ; Flavonoids ; analysis ; isolation & purification ; Ionic Liquids ; chemistry ; Primulaceae ; chemistry

Tyrosol, crenulatin and salidroside are the main active constituents of Rhodiola crenulata, with extensive pharmacological activities. In the study, grams of high purity tyrosol, crenulatin and salidroside were simultaneously separated from R. crenulata by the first time. Firstly, R. crenulata was extracted by 70% alcohol. Then, with the yields of three compounds as the index, the macroporous resin was optimized. At last, grams of high purity tyrosol, crenulatin and salidroside were isolated by D-101 macroporousresin, purified by column chromatography. Detected by HPLC, the purity of three compounds were higher than 98%. This method has the advantages of simple process and operation, less dosage of organic solvent, highly yield and reproducibility, suitable for the simultaneously preparation of tyrosol, crenulatin and salidroside.
Chemical Fractionation ; methods ; Chemistry, Pharmaceutical ; Chromatography, High Pressure Liquid ; Coumarins ; analysis ; isolation & purification ; Drugs, Chinese Herbal ; analysis ; isolation & purification ; Glucosides ; analysis ; isolation & purification ; Phenols ; analysis ; isolation & purification ; Phenylethyl Alcohol ; analogs & derivatives ; analysis ; isolation & purification ; Rhodiola ; chemistry

For further improving the extraction efficiency of microwave extraction, a microwave-assisted contijuous extraction (MACE) device has been designed and utilized. By contrasting with the traditional methods, the characteristics and extraction efficiency of MACE has also been studied. The method was validated by the analysis of the triterpenoids in Ganoderma lucidum. The extraction conditions of MACE were: using 95% ethanol as solvent, microwave power 200 W and radiation time 14.5 min (5 cycles). The extraction results were subsequently compared with traditional heat reflux extraction ( HRE) , soxhlet extraction (SE), ultrasonic extraction ( UE) as well as the conventional microwave extraction (ME). For triterpenoids, the two methods based on the microwaves (ME and MACE) were in general capable of finishing the extraction in 10, 14.5 min, respectively, while other methods should consume 60 min and even more than 100 min. Additionally, ME can produce comparable extraction results as the classical HRE and higher extraction yield than both SE and UE, however, notably lower extraction yield than MASE. More importantly, the purity of the crud extract by MACE is far better than the other methods. MACE can effectively combine the advantages of microwave extraction and soxhlet extraction, thus enabling a more complete extraction of the analytes of TCMs in comparison with ME. And therefore makes the analytic result more accurate. It provides a novel, high efficient, rapid and reliable pretreatment technique for the analysis of TCMs, and it could potentially be extended to ingredient preparation or extracting techniques of TCMs.
Chemical Fractionation ; methods ; Drugs, Chinese Herbal ; analysis ; isolation & purification ; Microwaves ; Reishi ; chemistry ; Terpenes ; analysis ; isolation & purification