TLC Identification of Yao Medicine Pileostegia tomentellal and Extraction Technology and Content Determination of Umbelliferone

[Objectives]To establish a TLC and content determination method of Pileostegia tomentellal,with umbelliferone as the indicator component.[Methods]TLC identification was performed by silica gel G thin layer plate with n-hexane-ethyl acetate(4:3)as the developing agent,and the plate was examined by UV lamp(365 nm).The umbelliferone content was determined by HPLC:Inertsil ODS-3 C 18 column(4.60 mm×250 mm,5μm);mobile phase acetonitrile-0.2%phosphoric acid gradient elution;detection wavelength 320 nm,flow rate 1.0 mL/min,column temperature 30℃,injection volume 10μL.[Results]The chromatogram of P.tomentellal showed the same color spot in the same position as that of reference medicinal material,and the spot was clear with good specificity.Umbelliferone showed a good linear relationship when the injection volume was 2.63-131.27μg/mL(R^(2)=0.9997).The average recovery of umbelliferone in the low,middle and high adding groups of P.tomentellal was 99.57%and the RSD was 2.15%.[Conclusions]The method can effectively identify Yao medicine P.tomentellal and accurately determine the content of umbelliferone in medicinal materials,which will provide a scientific basis for the development and utilization of medicinal resources of Yao medicine P.tomentellal.

Optimization of Extraction Process for Total Flavonoids from Penthorum chinense Pursh and Comparison of Their Contents from Different Parts

[Objectives]This study was conducted to optimize the extraction process of total flavonoids from Penthorum chinense Pursh and compare their contents from different parts.[Methods]Single factor and orthogonal experiments were designed to optimize the extraction process of total flavonoids from P.chinense Pursh with the volume fraction of ethanol,the ratio of material to liquid,heating reflux extraction time and extraction times as factors,and the content of total flavonoids as the index.A verification test was carried out.The optimized extraction process was adopted to compare the contents of total flavonoids from different parts of P.chinense Pursh.[Results]The best extraction process was extracting the powder of P.chinense Pursh for 2.0 h with 20 times of 55%ethanol by reflux twice.Under this condition,the contents of total flavonoids were 3.63%,8.90%,11.28%,and 4.36%from stems,leaves,flowers and whole grass of P.chinense Pursh,respectively.[Conclusions]The process is reasonable,feasible and stable,and can effectively extract total flavonoids from P.chinense Pursh.The contents of total flavonoids from different parts of P.chinense Pursh were quite different,and the value was higher in the leaves and flowers,so the proportions of leaves and flowers should be paid attention to in the industrial processing of P.chinense Pursh.

Determination of Chlorogenic Acid,Geniposide,Total Flavonoids and Total Triterpenes in Wulan-13

[Objectives]This study was conducted to establish a method for the determination of chlorogenic acid,geniposide,total flavonoids and total triterpenes in Wulan-13.[Methods]The contents of chlorogenic acid and geniposide were determined by HPLC,and the contents of total flavonoids and total triterpenes were determined by an ultraviolet spectrophotometer.[Results]There was a good linear relation between the mass of chlorogenic acid reference substance and the peak area in the range of 0.05-0.45μg,and the regression equation was Y=2524.1X+3.1943,(r=0.9998).A good linear relationship was found between the mass of gardenoside reference substance and the peak area in the range of 0.776-6.984μg,and the regression equation was Y=1670.5X+64.804,(r=0.9998).There was also a good linear relation between the mass of rutin reference substance and its absorbance in the range of 0.00808-0.04848 mg,and the regression equation was Y=12.916X+0.014,(r=0.999).The mass of oleanolic acid reference substance had a good linear relation with its absorbance in the range of 0.00418-0.0209 mg,and the regression equation was Y=51.89X-0.0839,(r=0.9991).[Conclusions]The content determination method is simple,reliable and reproducible,and suitable for controlling the contents of chlorogenic acid,geniposide,total flavonoids and total triterpenes in Wulan-13.

Determination of Salvianolic Acid B in Yiqi Huayu Prescription by HPLC

[Objectives]To determine the content of salvianolic acid B in Yiqi Huayu Prescription by HPLC.[Methods]The chromatographic column was ZORBAX Eclipse Plus C 18(4.6 nm×250 nm,5μm);the mobile phase was acetonitrile-0.1%phosphoric acid(21:79),the detection wavelength was 286 nm,the column temperature was 30℃,and the flow rate was 1.0 mL/min.A method for determination of salvianolic acid B in Yiqi Huayu Prescription was established.[Results]The linear relationship of salvianolic acid B was good in the range of 0.0214-0.4064 mg/mL.The regression equation was Y=5995.98984 X-0.07332,r=0.9999.The average recovery rate was 98.88%(RSD=1.6%).[Conclusions]The method is reliable,accurate and specific,and can be used for the determination of salvianolic acid B in Yiqi Huayu Prescription.

Determination of the Contents of Seven Chemical Components in Vidal Grape by Quantitative Analysis of Multi-components by Single Marker(QAMS)

[Objectives]This study was conducted to establish a method of quantitative analysis of multi-components by single marker(QAMS)for the simultaneous determination of such seven chemical components as gallic acid,epicatechin,catechin,ferulic acid,chlorogenic acid,rutin and caffeic acid in Vidal grape.[Methods]The high performance liquid chromatography was carried out using a COSMOSIL C18-MS-II column(4.6 mm×250 mm,5μm)with the mobile phase acetonitrile-2%acetic acid aqueous solution(gradient elution)at a flow rate of 1.0 ml/min.The detection wavelength was 280 nm,and the column temperature was 25℃.Using caffeic acid as an internal reference,the relative correction factors between it and other six to-be-detected components,and the contents of the seven components were calculated using the correction factors.The established was compared the results with the external standard method to verify the feasibility and accuracy of the method.[Results]The seven components had a good linear relationship in the ranges of 1.060-10.60,1.419-14.19,1.062-10.62,0.2950-2.950,0.1019-1.019,0.2014-2.014,and 0.1498-1.498μg,respectively,and the relative correction factors of gallic acid,epicatechin,catechin,ferulic acid,chlorogenic acid and rutin were 0.9760,0.7806,0.3277,1.640,1.161,2.778,respectively.There was no significant difference between the results of the QAMS method and the external standard method.[Conclusions]The QAMS method using caffeic acid as an internal reference is accurate and feasible,and provides a reliable method for the quality evaluation of Vidal ice grape.

Purification Process,Content Determination,Pharmacological Activity and Molecular Mechanism of Neogambogic Acid

Neogambogic acid is characterized by broad antitumor spectrum,good antitumor effect and low toxicity and side effects.This paper reviews the purification process,content determination and pharmacologic activity of neogambogic acid,in order to provide a theoretical reference for the research and application of neogambogic acid.

Determination of Total Flavonoids in Leaves of Tetracera asiatica

[Objectives] This study was conducted to determine and compare the contents of flavonoids in the leaves of Tetracera asiatica , an ethnic medicine from different habitats, in order to provide a basis for the quality control of its medicinal materials. [Methods] The flavonoid compounds in the leaves of T. asiatica were reflux-extracted in a water bath, and the total flavonoid content in T. asiatica was determined by ultraviolet-visible spectrophotometry. [Results] The total flavonoid content in T. asiatica leaves varied according to different habitats. The highest content was found in Gaofeng (19.41%) of Guangxi, followed by Huizhou (16.88%) of Guangdong and Hong Kong (16.76%). The lowest total flavonoid content was found in Shangcuntang (3.91%) of Bobai County, Guangxi, followed by Beiliu (4.15%), Guangxi. The total flavonoid contents in the samples ranged from 3.91% to 19.41%, with an average content of about 12.36%. [Conclusions] The UV spectrophotometry method is easy to operate, and has good repeatability, accurate detection results, and high reliability, and can be used for the determination of flavonoids in T. asiatica .

Research Progress on Purification Process Optimization and Content Determination of Zeaxanthin

At present,the purification process of zeaxanthin mainly includes organic solvent extraction,ultrasonic-assisted extraction and enzyme extraction,and the content determination technology mainly includes ultraviolet-spectrophotometry and high performance liquid chromatography.In this paper,the purification process and content determination technology of zeaxanthin in recent years are reviewed in order to provide ideas and theoretical basis for further research and application of zeaxanthin.

Determination of the Content of Five Active Components in Toad Skin

[Objectives] To establish a method for the determination of active components in toad skin. [Methods] HPLC method was used to determine the content of five active components (bufotalin, cinobufotalin, bufalin, cinobufagin and resibufogenin) in toad skin. [Results] Chromatographic conditions are as follows: Agilent ZORBAX SB-C 18 chromatographic column was used;acetonitrile (A)-0.3% glacial acetic acid (B) gradient elution (0-15 min, 28%A-54%A;15-35 min, 54%A-54%A) was conducted;the flow rate was 0.6 mL/min;the detection wavelength was 296 nm;the column temperature was 30 ℃;the sample size was 10 μL. Under the above conditions, the determination method of the five components can be established at one time. [Conclusions] The method was stable and reliable, and can provide experimental basis for the development and utilization of active ingredients in toad skin.

Study of Quality Standards of Xiao’er Qingre Enema Preparation in Hospitals

Objective:To establish the quality standards for the preparation of Xiao’er Qingre enema in hospitals.Method:Thin-layer chromatography(TLC)was used to identify Radix Isatidis and Glycyrrhizae in the prescription.The content of(R,S)-Goitrin was determined by high-performance liquid chromatography(HPLC).Results:In TLC identification,there was no interference between the negative controls of Radix Isatidis and glycyrrhizae,and the spots were well-separated.The HPLC results of(R,S)-Goitrin showed a good linear relationship between the peak area and concentration within the range of 0.476-95.2μg·mL-1(r=0.9999).Conclusion:The TLC and HPLC methods established in this experiment are simple,reproducible,and specific,making them suitable for the quality control Xiao’er Qingre enema preparation in hospitals.

Extraction Process and Content Determination of Caffeic Acid in Laggera alata from Different Production Areas of Guangxi

[Objectives] To establish a method for determining the content of Laggera alata( D. Don) Sch. Bip. Ex Oliv. using caffeic acid the target component,and to compare the content of caffeic acid in the medicinal materials of L. alata in different production areas of Guangxi.[Methods]The content was determined by Inertsil~ODS-3 chromatographic column C_(18)( 4. 60 mm × 250 mm,5 μm,mobile phase: acetonitrile-0. 1% phosphoric acid( 22∶ 78),detection wavelength: 320 nm,flow rate: 1. 0 m L/min,column temperature: 30℃,and injection volume: 10 μL. [Results] The caffeic acid showed a good linear relationship in the range of injection volume of 0. 025 92-0. 259 2 μg( R =0. 999 5). The average recovery rate was 98. 33%( RSD = 1. 85%). L. alata in different production areas of Guangxi contained the caffeic acid,and there was a great difference in the caffeic acid. L. alata in Baise had the highest content of caffeic acid,while that in Guilin had the lowest content of caffeic acid. [Conclusions]This method can accurately determine the content of caffeic acid and is expected provide a scientific basis for the development and utilization of herbal medicine L. alata.

Chemical Analysis Method for Magnesia and Magnesia-Alumina Refractories——Gravimetric-Molybdenum Blue Photometric Method for Determination of Silicon Dioxide Content

This standard specifies the gravimetric-molybdenum blue photometric method for determination of silicon dioxide content.

Thin-layer Identification,Extraction Process and Content Determination of Chlorogenic Acid in Laggera alata(D.Don)Sch.Bip.ex Oliv.

[Objectives]This paper aims to establish thin-layer identification and content determination method for Laggera alata(D.Don)Sch.Bip.ex Oliv.with chlorogenic acid as the index component and compare the content of chlorogenic acid in L.alata from different places in Guangxi.[Methods]Silica gel GF254 thin-layer plate was used for identification under an ultraviolet lamp(365 nm),with butyl acetate-formic acid-water(V∶V∶V=7∶2.5∶2.5)as a developing agent.The content of chlorogenic acid was determined under the following chromatographic conditions:column,Inertsil ODS-3 C18 column(4.60 mm×250 mm,5μm);mobile phase,methanol-0.1%phosphoric acid(28∶72);detection wavelength,329 nm;flow rate,1.0 mL/min;column temperature,25℃;and injection volume,10μL.[Results]Chlorogenic acid can be detected by thin layer chromatography with clear spot and good specificity.Chlorogenic acid showed a good linear relationship in the injection amount range of 0.099-0.99μg(R^(2)=0.9999).The content of chlorogenic acid in L.alata varied greatly among the 10 different producing areas in Guangxi.L.alata produced in Dee Township,Longlin,Baise,Guangxi showed the highest chlorogenic acid content,and that produced in Shangsi County and Pingle County showed the lowest chlorogenic acid content.[Conclusions]This method can effectively identify L.alata and accurately determine the content of chlorogenic acid,thereby providing a scientific basis for the development and utilization of L.alata resources.

Study on Determination of Tanshinones in Compound Danshen Tablets

[ Objective ] This study was conducted to improve quality standard of Compound Danshen tablets. [ Method] Tanshinones in Compound Danshen tab- lets were determined by HPLC method. [ Result] A good linear relationship was found in the range of 0.10 -0.50 μg, and the average recovery rate was 100.59% （RSD = 1.38% ）. [ Conclusion] The method is simple, rapid and reproducible, and could be used as a method for quality control of Compound Danshen Tablets.

Content Determination of Total Flavonoids from Paulownia fortunei Flower

[Objectives]The research aimed to explore the determination method for content of total flavonoids from Paulownia fortunei flower.[Methods]Rutin was taken as control.By comparing absorption characteristics of total flavonoids in NaNO_(2)-Al(NO_(3))_(3)-NaOH and AlCl_(3) chromogenic system,an appropriate method for the determination of total flavonoids from P.fortunei flower was screened,and the method was verified by methodology.On the basis of single factor experiment,the coloration time of the method was optimized by orthogonal experiment.[Results]NaNO_(2)-Al(NO_(3))_(3)-NaOH chromogenic system was more suitable for the determination of total flavonoids from P.fortunei flower,and the adding standard recovery was between 99.2%and 105.5%,and RSD was 2.18%,with better repeatability,precision,stability and accuracy.The optimized coloration time of NaNO_(2),Al(NO_(3))_(3) and NaOH was 6,6,and 10 min.Under the condition,average content of total flavonoids from P.fortunei flower was 3.78%,and RSD was 2.05%.[Conclusions]The optimized NaNO_(2)-Al(NO_(3))_(3)-NaOH chromogenic method is simple,rapid,and accurate,and could be used as a method for the determination of total flavonoids from P.fortunei flower.

Determination of Polydatin in Rat Serum and Its Changes by UPLC Method

[Objectives]To establish a UPLC-UV method for the determination of polydatin in the serum of Wistar rats.[Methods]Acquity UPLC BEH shield RP18 column(1.7μm,2.1 mm×100 mm,Waters Corporation,USA)was used as the analytical column,acetonitrile-water(55∶45)was used as the mobile phase,the flow rate was 0.5 mL/min,and the column temperature was 30℃and the detection wavelength was 306 nm.[Results]The linear range of the established serum sample analysis method was 1.0-20.0μg/mL,and the correlation coefficient was r=0.9994;the intraday and interday RSD of Wistar rat serum was less than 3.0%,and the accuracy was higher than 90%.[Conclusions]This method is sensitive,accurate,and rapid.It is suitable for monitoring the concentration of polydatin in serum after intragastric administration,and can also be used for pharmacokinetics and bioavailability studies.

Determination of the Content of Gastrodin in Jingtianshenma Tablets by High Performance Liquid Chromatography

[Objectives]The research aimed to establish a high performance liquid chromatography method for the content determination of gastrodin in Jingtianshenma Tablets.[Methods]A phenomenex Luna C18(250 mm×4.6 mm,5μm)column was used;the mobile phase was acetonitrile-0.05%phosphoric acid solution(3∶97);the detection wavelength was 220 nm,and the column temperature was set at 25℃.[Results]Gastrodin showed a good linear relationship in the range of 0.0984-0.5904μg with the peak area,and regression equation was Y=2000000X-51999(r=0.9999).The limits of detection and quantification for gastrodin were 2.50 and 4.20 ng respectively,and the average recovery rate was 95.95%.[Conclusions]This method is sensitive,accurate and reproducible,with good linearity,and it is suitable for the content determination of gastrodin in health food Jingtianshenma Tablets.

Determination of the Content of Astragaloside IV in Yikangshu Granules by High Performance Liquid Chromatography

[Objectives]The research aimed to establish a high performance liquid chromatography method for the content determination of astragaloside IV in Yikangshu Granules.[Methods]Kromasil 5μm C18(2),100 A,250 mm×4.6 mm was used;the mobile phase was acetonitrile-water(32∶68);flow velocity was 1.0 mL/min;the temperature of evaporator and sprayer was 80 and 30℃;the column temperature was set at 30℃,and injection volume was 20μL.[Results]Astragaloside IV showed a good linear relationship in the range of 1.01-10.14μg with the peak area,and regression equation was lgY=1.7728lgX+1.597(r=0.9999).The limit of detection for astragaloside IV was 1.96 ng,and the average recovery rate was 95.31%.[Conclusions]This method is sensitive,accurate and reproducible,with good linearity,and it is suitable for the content determination of astragaloside IV in health food Yikangshu Granules.

Establishment of a Method for the Determination of Emodin in Wudajiangjun Liquor

[Objectives]To establish a method for the determination of emodin in Wudajiangjun liquor,a hospital preparation.[Methods]A high-performance liquid chromatography(HPLC)method for the determination of emodin in Rhizoma Polygontum Cuspidatum in hospital preparation Wudajiangjun liquor was established.Using HPLC method,octadecylsilane chemically bonded silica gel was used as filler for the chromatographic column[Inertsil-C 18 chromatographic column(5μm,4.6 mm×250 mm)].Methanol-0.1%phosphoric acid water(76∶24)was used as mobile phase.The flow rate was 1.0 mL/min,the column temperature was 30℃,the detection wavelength was 254 nm,and the injection volume was 10μL.[Results]The content of emodin in Wudajiangjun liquor was determined by reversed-phase high performance liquid chromatography(RP-HPLC).When the injection volume of emodin was in the range of 5.45-54.5μg/mL,there was a good linear relationship between the injection volume and the peak area.The regression equation is Y=42.952-15.068(r=0.9998),the average recovery rate is 98.23%,and RSD=1.45%.[Conclusions]A method for the determination of emodin in Wudajiangjun liquor by HPLC was established.This method can be used as a quality control method for Wudajiangjun liquor with high accuracy and good repeatability,which lays a foundation for the quality control of the medicinal liquor.

Determination of Volatile Oil and Ferulic Acid in Different Parts of Wild Ferula sinkiangensis K. M. Shen and Ferula fukanensis K. M.Shen Cultivars

[Objectives] To increase the reserves distribution and planting area of Ferula resources,protect wild Ferula resources,make comparative analysis on wild and cultivated varieties of Ferula medicinal materials,and provide references for quality evaluation of Ferula herbs collected from cultivation environment. [Methods] Volatile oil determination and high performance liquid chromatography were used to measure volatile oil and ferulic acid in different parts of wild and cultivated varieties of Ferula. [Results] In the volatile oil measured from artificially pressed Ferula lipid,wild varieties in different places conformed to the pharmacopoeia standard( volatile oil content ≥10%); in cultivated varieties,F. fukanensis K. M. Shen and F. sinkiangensis K. M. shen reached the pharmacopoeia standard. According to measurement results of ferulic acid,the ferulic acid content of roots and leaves of Altay,Fukang,and Yining cultivars were higher than that of wild varieties. [Conclusions]The ferulic medicinal herbs collected from artificial cultivation environment have considerable prospect,and many parts of Ferula herbs can be used for raw materials for preparation of extracts.