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.

TLC Identification and Extraction Process of Rubiasin-1-methyl Ether from Yao Medicine Chuanlianzhu

[Objectives]To establish a thin-layer chromatography(TLC)method for the determination of rubiadin-1-methyl ether in Yao Medicine Chuanlianzhu(Damnacanthus giganteus).[Methods]A silica gel G thin-layer plate was adopted for TLC.Petroleum ether(60-90℃)-chloroform-methanol-water(7:15:3:1)was used as the developing solvent and inspected under ultraviolet lamp(365 nm).The content was determined by Inertsil ODS-3 C 18 column(4.60 mm×250 mm,5μm),mobile phase:acetonitrile-0.2%phosphoric acid gradient elution,detection wavelength 277 nm,flow rate 1.0 mL/min,column temperature 30℃,injection volume 10μL.[Results]The spots of 10 Chuanlianzhu samples from different origins showed the same color at the same position as the control,and the spots were clear and specific.The injection volume of rubiadin-1-methyl ether showed a good linear relationship in the range of 2.90-145μg(R=0.9996).The average recovery rate of rubiadin-1-methyl ether in the low,medium and high dose groups of Yao Medicine Chuanlianzhu was 98.72%,and RSD=1.78%.[Conclusions]This method can effectively identify Yao Medicine Chuanlianzhu medicinal materials and accurately determine the content of rubiadin-1-methyl ether in the medicinal materials.It provides a scientific basis for the development and utilization of Yao Medicine Chuanlianzhu medicinal resources.

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.

Colorimetric determination of nanomolar concentrations of silicate in natural waters after liquid-liquid extraction using methyl isobutyl ketone

A sensitive solvent extraction method for the determination of nonamolar concentrations of silicate in natural waters is developed. According to the traditional aqueous silicate method, silicomolybdenum blue formed by the reaction between silicate and ammoni- um molydate and reduced by metol-sulfite reagent is extracted by methyl isobutyl ketone. The absorbance can be enhanced substantially up to 10-folds. The detection limit of silicate is 8 nmol/dm^3 , which is one tenth smaller than the traditional method, with the precision of 4.0% at a silicate level of 50 nmol/dm^3 and 3.2% at a silicate level of 6 μmol/dm^3. Comparing the calibration curves in the distilled water and seawater, it can be seen that the salt effect also exists in the extraction method. However, the salt effect is a linear function of the salinity and can be corrected by simple calibration. The proposed method is successfully applied to the determination of silicate in natural waters. Natural concentrations of arsenate, arsenite and phosphate cause negligible interference.

Extraction Process and Content Determination of Total Flavonoids in Ginkgo( Ginkgo biloba L. ) Leaves

[Objectives]This study was conducted to study the extraction process and the content determination of flavonoids in ginkgo( Ginkgo biloba L.) leaves.[Methods]Ethanol extraction and methanol extraction of total flavonoids in ginkgo leaves were studied,and the optimal extraction conditions for flavonoids were determined by orthogonal test; and with quercetin as reference substance,total flavonoid content in ginkgo leaves was determined by UV spectrophotometry.[Results]The optimal extraction process was 4 h of Soxhlet extraction with methanol; and the total flavonoid contents had a good linear relation in the range of 0. 006 5-0. 039 mg/ml( R^2= 0. 999 9),the average content was stabilized at 1. 135%,and the average recovery of the method was 102. 0%. [Conclusions]This study selected the optimal extraction process for total flavonoids in ginkgo leaves. The test method is simple with high accuracy and precision,and is suitable for the extraction and determination of total flavonoids in ginkgo leaves.

Determination of polycyclic aromatic hydrocarbons with supercritical fluid extraction and chromatography（SFE／SFC）

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Simultaneous Determination of Bisphenols and Alkylphenols in Water by Solid Phase Extraction and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

To establish an analytical method for determination of four bisphenols （BPA, BPB, BPF, and BPS） and two alkylphenols （4-n-OP, 4-n-NP） in water by ultra performance liquid chromatography- tandem mass spectrometry （UPLC/MS/MS）. The water samples were extracted and condensed with solid-phase extraction （SPE） using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.

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.

Extraction Technology of Total Flavonoids from Pueraria lobata (Willd.) Ohwi and Content Determination of Pueraria lobata (Willd.) Ohwi at Different Altitudes

[Objectives]To optimize the extraction technology of total flavonoids from Pueraria lobata( Willd.) Ohwi. [Methods]The ultraviolet-visible spectrophotometry was used to determine the content of total flavonoids in Pueraria lobata( Willd.) Ohwi. With the puerarin as index,the reflux extraction and single factor test were employed to investigate the effects of temperature,time,ethanol concentration and solid-liquid ratio on the content of total flavonoids in Pueraria lobata( Willd.) Ohwi,respectively. Under the optimal extraction technology,the content of total flavonoids in Pueraria lobata( Willd.) Ohwi at different altitudes was determined.[Results] The optimum extraction process was as follows: 70%ethanol; solid-liquid ratio of 1∶ 30; 1 h reflux extraction. Under these conditions,the extraction rate of flavonoids in Pueraria lobata( Willd.) Ohwi was 11. 48%,the total flavonoids content of different kudzu parts was in the order of roots > stems > leaves,and the total flavonoids content of the sample at about an altitude of 1000 m was significantly higher than at the altitudes of 1400 m and 1700 m.[Conclusions]It was suggested that the Pueraria lobata( Willd.) Ohwi should not be cultivated as medicinal plant in too high mountains,and the stems and leaves of Pueraria lobata( Willd.) Ohwi could be used as raw materials for extracting total flavonoids.

Optimization of Extraction Process and Content Determination of Total Flavonoids from Sanguisorbae Radix and Carbonized Sanguisorba Root by Orthogonal Experimental Design

[Objectives] To optimize the extraction process of total flavonoids from Sanguisorbae Radix and carbonized Sanguisorba root,compare quality of different batches of Sanguisorbae Radix,study the effects of processing on the content of flavonoids,and provide scientific basis for reasonable utilization of Sanguisorbae Radix. [Methods] Test samples were prepared by heating,refluxing,and extraction,the extraction process was optimized by orthogonal experiment design,color was developed by NaNO_2-Al( NO_3)3-NaOH,and total flavonoids were measured by UV method at the wavelength of 510 nm. [Results] The linear relationship of rutin was excellent in the concentration range of 0. 1248 mg/mL-0. 5712 mg/mL,R^2= 0. 9997; the average recovery was 99. 67% and the RSD was 0. 70%. The optimum extraction conditions were as follows: the volume fraction of ethanol was 50%,the extraction temperature was 90℃,the extraction time was 90 min,and the solid-to-liquid ratio was 1∶ 20( g/mL). [Conclusions] After optimization of the extraction process,the extraction rate of total flavonoids in samples of Sanguisorbae Radix was significantly increased; there was certain difference in the content of total flavonoids between different batches of Sanguisorbae Radix and processed products; the total flavonoids significantly declines in carbonized sanguisorba root,and the influence of processing on its curative effect was to be further studied.

Solid-liquid Extraction Spectrophotometric Determination of Copper with 2,9-dimethyl-1,10-phenanthroline

Solid liquid extraction of copper ion (I) with 2, 9-dimethyl-1, 10-phenanthroline (neo-cuproine, DMP) into molten naphthalene followed by chloroform spectrophotometric determination has been studied experimentally. The ternary complex Cu(I)-DMP-ClO4 was extracted quantitatively into molten naphthalene in the range of pH from 5 to 6 at 85 C-. Absorbance was spectrophotometrically determined at 459 nm against the reagent blank after the solid naphthalene layer was anhydrously dissolved in chloroform. Beer's law is obeyed over a concentration range of 0.5-70 mug/mL. The molar absorptivity and Sandell's sensitivity are 1.0x10(4) L/(mol(.)cm) and 0.0099 mug(.)cm(2) respectively. In addition, the various conditions on determination and the interference of coexisted ions were discussed, and the method was applied to the determination of copper ion both in tea samples and cadmium sulfate reagents. The results are in good agreement with those obtained by ICP AES method.

Extraction Process and Content Determination of Caffeic Acid in Zhuang Medicine Cryptolepis buchananii

[Objectives]To establish a method for determining the content of caffeic acid in Zhuang Medicine Cryptolepis buchananii.[Methods]The content of caffeic acid in C.buchananii leaves was determined by high performance liquid chromatography(HPLC).[Results]The results of HPLC determination showed that the RSD values were less than 3%,and the content of caffeic acid in 10 batches of C.buchananii leaves was in the range of 0.0965%-0.4772%.[Conclusions]This method is accurate and reliable,has good linear relationship and high precision,and can be used for quality evaluation of C.buchananii.

Technical Study on Extraction of Procyanidins in Lycium ruthenicum Murr. Using Sub-critical Fluid 1,1,1,2-Tetrafluoroethane( R134a)and Content Determination from Different Producing Areas

[Objectives] To study the optimal conditions for extracting procyanidins fromLycium ruthenicum Murr. with sub-critical fluid R134 a( 1,1,1,2-tetrafluoroethane) in 1 L extraction kettle. [Methods]Taking the extraction rate of procyanidins as an indicator,the influence of pressure,temperature,and extraction time on extraction rate of procyanidins fromL. Ruthenicum Murr. was studied by single factor experimental methods and orthogonal array design. [Results]The order of factors affecting extraction rate of procyanidins was extraction temperature > extraction pressure > extraction time. The optimum extraction conditions were as follows: the extraction rate of procyanidins fromL. ruthenicum Murr. was the highest with extraction pressure of 1. 2 MPa,extraction temperature of 50℃ and extraction time of 90 min. The content of procyanidins in L. ruthenicum Murr. from different producing areas was determined by vanillin-HCl method under the optimal conditions. [Conclusions] The method has the advantages of easy operation,good selectivity,low extraction temperature and high extraction efficiency,which is suitable for extraction of procyanidins in L. ruthenicum Murr.

Micelle Mediated Extraction of Iron and Its Determination in Geological, Geochemical, Hydrogeochemical, Biogeochemical and Process Solutions

Iron irrespective of its valency states forms bluish 1:1 cationic, bluish-violet 1:3 neutral and purple 1:3 anionic complexes with 2,3-dihydroxynaphthalene, at pH 2 - 3, 4 - 5 and 8 - 10, respectively. The cationic bluish complex is highly insensitive and not extractable in organic solvents. Similarly, the bluish violet 1:3 neutral complex is of moderate sensitivity, and it is extractable in organic solvents with reduced sensitivity. The purple 1:3 anionic complex is as such not extractable in any organic solvents. However, in the surfactant medium of the cationic surfactant, cetyltrimethylammonium bromide it is extractable in organic solvents with enhanced sensitivity. The 1:3 anionic complex which is extractable in organic solvents as an ion associate in the presence of cetyltrimethyl ammonium bromide is chosen for application to Silicate rocks, Minerals, Soils, Stream sediments, Concentrates, Tobacco leaves, Cigarettes and Waters, for accurate and sensitive determination of iron owing to facile extraction of iron, enhanced sensitivity high selectivity and better reproducibility of results. The present paper describes a systematic study on the development of an extraction spectrophotometric method for the determination of iron in samples of diverse matrices.

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.

THE STUDY ON THE WATER SOLUBLE PEPTIDES IN PAPAVER SOMNIFERUM POLLEN EXTRACTION,PURIFICATION,SEQUENCE DETERMINATION AND SYNTHESIS

Four peptides PSPP1,PSPP2,PSPP3 and PSPP4 were purified from the water-extract of Papaver somniferum pollen.Their sequences,with 21,17,13 and 16 amino acid residues respectively,have been determined by Edman degradation-N-terminal dansylation.PSPP2, PSPP3 and PSPP4 were synthesized using solid phase method.The immunopromotive activities of PSPP1,PSPP2,PSPP3,PSPP4 and the initially separated sample PSPP have been also observed by the methods of counting erythrocyte rosette forming cells(ERFC) and T-lymphocyte transformation test in vitro.

Determination of Manganese in Tap Water by a New Extraction-Photometric Method

The heteroligand complex of manganese with 1,10-phenantroline and o-nitrobenzolazosalicylic acid has been investigated by spectrophotometric method. The condition of complexing and extraction, physical-chemical and analytical characteristics of this complex have been found. Complex formation is observed in the pH range 5 - 11. Extraction constant was found as 5.3 × 1012, stability constant was found as lgβK = 9.03?± 0.03. Molar absorptivity is ε = (1.36 ± 0.08) × 104 l·g﹣1·cm﹣1. Beer's law is obeyed in the range of 1.0 - 22.5 μkg manganese (II). The extraction-photometric methods of manganese determination have been worked out. The influence of diverse ions on determination of manganese (II) has been studied. The proposed method was applied successfully to determine amount of manganese in tap water.

Alizarine Yellow R as Reagent of the Determination of Manganese by Extraction-Photometric Method

4,7-diphenyl-1,10-phenantroline from heterocyclic diamines and alizarine yellow R from chromogenic reagents have been used for spectrophotometric determination of manganese in the form of heteroligand manganese complex. The complex formation and extraction condition, physical-chemical and analytical characteristics of this complex have been established. 5.5 - 11.0 pH range is observed as complex formation pH range. Extraction and stability constants were accordingly found as Kext = 8.32 × 1014 and lgβK = 7.2 ± 0.1. Molar absorptivity is ε = (2.27± 0.08) × 104 l·g-1·cm-1. In the range of 0.5 - 23.0 μkg manganese (II) Beer’s law is obeyed. The extraction-photometric methods of manganese determination have been worked out. The strangers ions influence on determination of manganese (II) has been studied. To determine amount of manganese in eggplant the proposed method was applied successfully.

Extraction Process and Quality Standard of Danshen Jianxin Capsules

[Objectives]This study was conducted to establish the quality standard of Danshen Jianxin Capsules.[Methods]Orthogonal design was adopted to optimize the water extraction process by taking the amount of water added,extraction time and extraction times as factors,and the content of tanshinone I as the index.Salviae Miltiorrhizae,Notoginseng Radix Et Rhizoma and Radix Astragali in the capsules were qualitatively identified by TLC,and the content of tanshinone I in the capsules was determined by HPLC.[Results]The best water extraction process included the steps of adding 12 times of water each time,extracting the materials twice,for 1 h each time.In TLC identification,the test samples showed spots of the same color at the positions corresponding to tanshinone II A,ginsenoside Rg1,notoginsenoside R1 and astragaloside IV reference samples.[Conclusions]Danshen Jianxin Capsules was prepared by the water extraction method,which is characterized by high efficiency and being suitable for mass production.The quality control method is reliable,fast and accurate,which can effectively control the quality of the product.

Extraction Process of Zhuang Medicine Fumigation Lotion

[Objectives]To establish the extraction process and quality standard method of Zhuang medicine fumigation lotion.[Methods]The orthogonal design method was employed to optimize the water extraction process with the amount of water added,decocting time and extraction times as factors,and syringin content and dry extract yield as indexes.The content of syringin was determined by high performance liquid chromatography.[Results]The best water extraction process was:soaking in water for 1 h,decocting twice,added 10 times the amount of water each time,decocting for 1 h.The average content of syringin in 3 batches was 0.98 mg/g,and the average dry extract yield was 26.07%.[Conclusions]The project adopts water extraction method to prepare Zhuang medicine fumigation lotion,which has the characteristics of high efficiency and suitable for large-scale production.The quality control method is reliable,rapid and accurate,and can effectively control the quality of the lotion.