Optimization of Extraction Technology of Volatile Oil and Inclusion Technology in Quhan Zhufeng Granules / 中国药房

OBJECTIVE： To establish the method for content determination of ligustilide and to optimize the extraction technology of volatile oil and inclusion technology in Quhan zhufeng granules. METHODS： HPLC method was adopted. The determination was performed on Waters C18 column with mobile phase consisted of methanol-water （70 ∶ 30， V/V） at the flow rate of 1 mL/min. The detection wavelength was set at 327 nm， and the column temperature was 30 ℃. The sample size was 10 μL. Using yield of volatile oil and the content of ligustilide as index， with soaking time， the amount of adding water and extraction time as factors， the extraction technology was optimized by orthogonal test. Using inclusion rate， the yield of inclusion compound and yield of volatile oil as index， with ratio of volatile oil to β-cyclodextrin， inclusion temperature and inclusion time as factors， the inclusion technology of volatile oil was optimized by orthogonal test. RESULTS： The linear range of ligustilide was 0.4-4 μg（r＝0.999 9）； RSDs of precision， stability and reproducibility tests were all lower than 2％ （n＝6）. The recoveries were 96.75％-102.03％（RSD＝2.06％，n＝6）. The optimal extraction technology of volatile oil included 10-fold water （mL/g）， soaking for 15 min， extracting for 8 h. Average yield of volatile oil was 0.310 7％， and average content of ligustilide was 0.418 0 mg/g. The optimal inclusion technology of volatile oil included ratio of β-cyclodextrin and volatile oil was 1 ∶ 8 （mL/g）； inclusion temperature was 50 ℃； inclusion time was 3 h. Average inclusion rate was 69.43％， and the yield of inclusion compound was 58.89％； the yield of volatile oil was 14.15％. CONCLUSIONS： Established determination method is simple， accurate and stable. The optimal extraction technology of volatile oil and inclusion technology are stable and feasible.

Optimization of the Purification Process of Yiqi Guben Granules with Multiple Indexes / 中国药房

OBJECTIVE:To optimize the purification process of the extract from Yiqi guben granules. METHODS:The purifi-cation effect of the process was investigated with transfer rate of polysaccharide,calycosin glucoside and dry paste as evaluation in-dexes,using ZTC1+1 type Ⅱ,and shell poly sugar and 95% ethanol as clarifying agents. The purification process of the extract from Yiqi guben granules was optimized by orthogonal test using the ratio of material to liquid,the amount of clarifying agent and standing time as factor. The validation test was conducted. RESULTS:Selecting ZTC1+1 type Ⅱ as a clarifying agent,the best trans-fer rate of effective component had been obtained;optimal purification process was as follows as the ratio of material to liquid 1:2, the ratio of ZTC1+1 type Ⅱ A liquid 5%,the ratio of B liquid 10%,standing time of 5 h. The results of verification test showed transfer rates of dry paste in 3 tests were 71.54%,70.98%,69.21%,respectively;those of polysaccharide were 82.55%, 81.78%,82.15%,respectively;those of calycosin glucoside were 91.92%,92.34%,91.58%,respectively (all RSD≤1.72%, n=3). CONCLUSIONS:The optimized purification process is effective,stable and practical,and can be used for the purification of the extract from Yiqi guben granules.

Optimization of Prescription of Flaxseed Lignans Sustained-release Tablets by Central Composite Design-response Surface Methodology / 中国中医药信息杂志

Objective To optimize the prescription of flaxseed lignans sustained release tables by central composite design-response surface methodology.MethodsWith HPMC, EC and starch dosage as factors, and flaxseed lignans in 2, 6 and 12 h of cumulative release as evaluation indexes, central composite design-response surface optimization method was used to conduct prescription optimization experiments, and optimized prescription analysis was carried out.Results The optimal prescription of flaxseed lignans sustained release tables was as following: HPMC dosage was 43%; EC was 26%; starch content was 17%. Optimized index forecast values were very close to the observed values. In vitro release test of three selected optimal formulations indicated that there existed high approximation between the observed and estimated values.Conclusion It shows that the established model is suitable for flaxseed lignans sustained release tables, which can be used in the optimization of the prescription of flaxseed lignans sustained release tables.

Effects of chronotherapy on neutrophils in breast cancer patients / 中国实用护理杂志

Objective To investigate the effect of chronotherapy (chemotherapy plus timely medication) on neutrophils in breast cancer patients with neoadjuvant chemotherapy.Methods Fifty breast cancer patients with neoadjuvant chemotherapy were selected from 2011 to 2014 and divided into chronotherapy group and conventional treatment group (conventional group) by random number table method with 25 cases each.Conventional group received conventional neoadjuvant chemotherapy and conventional drug treatment.Chronotherapy group received neoadjuvant chemotherapy combined with chronochemotherapy and timely medication treatment,and applied clinical nursing care pathway.Both groups were conducted three cycles of chemotherapy,three weeks after the first and the second chemotherapy,the results of routine blood and liver function were compared in patients between two groups.The number of readmission and fever because of agranulocytosis were calculated.Results The two groups of patients were successfully completed three cycles of chemotherapy,after the first cycle of chemotherapy,the neutrophil was (4.40 ± 2.20)x109/L in chronotherapy group,and (3.18 ± 1.35) × 109/L in conventional group;after the second cycle of chemotherapy,the neutrophil was (3.95 ± 1.58) × 109/L,and (2.83 ± 1.49) x 109/L in conventional group,the two groups were statistically significant,t=2.375,2.563,P ＜0.05.Two cases needed readmission in chronotherapy group during chemotherapy,accounting for 8％(2/25),much lower than conventional group of 8 cases accounting for 32％(8/25).Conclusions The use of chronotherapy in breast cancer chemotherapy has less neutropenia,mild side effects of bone marrow suppression.It is an effective and safe viable option.

Study on Quality Standard for Biqing Suppository / 中国中医药信息杂志

Objective To establish a quality standard for Biqing Suppository. Methods Rhizoma Dioscoreae Septemlobae, Rhizoma Acori Tatarinowii, Radix Et Rhizoma Salviae Miltiorrhizae and Cortex Phellodendri Chinensis were qualitatively identified by TLC method. The content of berberine hydrochloride in Biqing Suppository was determined by HPLC method. The chromatographic column was Waters C18 (250 mm×4.6 mm, 5 μm);the mobile phase was acetonitrile∶water (0.2%phosphoric acid-0.02%three triethylamine)=25∶75;the flow rate was 1 mL/min;the detection wavelength was 265 nm. Results The spots of qualitative identification method were clear without interference. Berberine hydrochloride had good linear relationship in the range of 0.235-9.40 μg;the regression equation was Y=40 033 998.176 3X-85 021.2, r=0.999 7;the average recovery rate was 99.16%, RSD=3.45%. Conclusion The method is simple, flexible and reproducible, which can be used as the quality control standard for Biqing Suppository.

Phamacokinetic study of bergapten in rats plasma by LC-MS/MS / 中国中药杂志

<p><b>OBJECTIVE</b>To determine bergapten's concentration in plasma and observe its pharmacokinetics in rats using a combined LC-MS/MS analytical method.</p><p><b>METHOD</b>Blood samples were separated on a Hypersil ODS column (4.6 mm x 250 mm, 5 mm) at a temperature of 30 degrees C, and mobile phase consisted of water and methanol (22.5: 77.5) at a flow rate of 0.8 mL x min(-1).</p><p><b>RESULT</b>The methodological study showed a good linear relationship of 8.12-162.4 g x L(-1) (r = 0.9999). The inner and inter-days relative standard deviations were both less than 10% , indicating legitimate precise and accuracy to the requirement of biological sample analysis.</p><p><b>CONCLUSION</b>The method is suitable for in vivo quantitative analysis for bergapten due to its accuracy, sensitivity and specificity. The pharmacokinetic process in rats forms a two-compartment model with first-order absorption.</p>

Quantification of six bioactive compounds in Zhenqi Fuzheng preparation by high-performance liquid chromatography coupled with diode array detector and evaporative light scattering detector / 药物分析学报

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.

Quantification of six bioactive compounds in Zhenqi Fuzheng preparation by high-performance liquid chromatography coupled with diode array detector and evaporative light scattering detector / 药物分析学报

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.

Evaluation preparation technology of Xiaochaihu granules using fingerprint-peak pattern matching / 药物分析学报

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.

Simultaneous determination of five active components in compound preparation of Dangguishuan by high-performance liquid chromatography / 中国中药杂志

<p><b>OBJECTIVE</b>To develop a HPLC method for determination of matrine, oxymatrine; ferulic acid, L-shikonin and beta, beta-dimethylacrylshikonin in compound preparatioti of Dangguishuan.</p><p><b>METHOD</b>The chromatogtaphic separation was performed on a Kromasil ODS C18 column (4.6 mm x 250 mm, 5 microm) maintaining at 30 degrees C during the whole process. The mobile phase consisted of methanol and 0.1% triethylamine aqueous solution (adjusted with phosphoric acid, pH 3) at a flow rate of 1.0 mL x min(-1). The detection wavelength was set at 220 nm for matririne and oxymatrine, 316 nm for ferulic acid, 516 nm for L-shikonin and beta, beta-dimethylacrylshikonin, respectively.</p><p><b>RESULT</b>All the compounds showed good linearity (r > 0.9996) in the range of the test concentrations, and the average recoveries of the method is betwuen 96.92% and 102.22%, RSD < 3.1%.</p><p><b>CONCLUSION</b>The method is proved to be credible, sensitive, accurate and repeatable. It can be applied to determine of matrine, oxymatrine, ferulic acid, L-shikonin and beta, beta-dimethylacrylshikonin in compound preparation of Dangguishuan simultaneously, and provide a basal method of quality control to this preparation and other relative preparations.</p>