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.

Co Content Dependence of Crystal Structure and Specific Magnetization of Fe_(1-x)Co_x-SiO_2 Granules Prepared by Sol-Gel Method

The Co content dependence of crystal structure and specific magnetization of Fe1-xCox-SiO2granular solid prepared by the sol-gel method have been studied. It is found that the crystal structure, Iattice parameter and specific magnetization of the FeCo alloy particles depend on the Co content.

HPLC Method for Determination of Content of Total Flavonoids from Ginkgo (Ginkgo biloba L.) Leaves

[Objectives]This study was conducted to determine the content of total flavonoids in ginkgo ( Ginkgo biloba L.) leaves.[Methods]The content of total flavonoids from ginkgo leaves was determined by reversed phase-high performance liquid chromatography (RP-HPLC).The flavonoid glycosides were first extracted with methanol,and hydrolyzed with hydrochloric acid solution to prepare a test solution.Platisil ODS C18 column (150 mm×4.6 mm,5 μm) and the mobile phase V methanol ∶ V water (0.4% phosphoric acid solution)=85∶ 15 were selected for HPLC separation.The HPLC separation was performed with the column at a column temperature of 25℃ using the mobile phase at a flow rate of 1 ml/min.The sample size was 10 μl,and detection was performed with an Agilent HPLC ultraviolet detector at 360 nm.[Results]The reference substance,quercetin,had good linearity in the range of 0.002 6-0.052 0 g/L,with a correlation coefficient of 0.999 7;and the RSD was 1.26%.[Conclusions]The determination method has rapid and simple operation with accurate results and is good in repeatability.This method is suitable for the determination of content of total flavonoids in ginkgo leaves.

Identification of variety of rice and determination of content of each rice in mixtures of two rices by nonlinear chemical analysis

Fingerprints of two varieties of rice and their mixtures were investigated by a nonlinear chemical reaction system consisting of rice components,sodium bromate,manganese sulfate,sulfuric acid and acetone.The variety of rice was identified by the visual characteristic of fingerprint and system similarity pattern recognition,and the content of each variety of rice in the mixture was determined by the quantitative information of fingerprint.The results show that nonlinear chemical analysis may be used to exactly identify the variety of pure rice and to accurately determine the content of each variety of rice in the mixture,indicating the method is simple and convenient.

Amylose Content and Starch Granule Size in Rice Grains are Affected By Growing Season

Amylose content and starch granule size in grains influence rice quality,which differs between the early(ES)and late season(LS).The objective of this study was to determine the variation of amylose content and starch granule size between seasons and find the main reasons(e.g.,temperature and solar radiation)for the observed variation.Field experiments with six rice varieties(three high and three low amylose content rice)planted in the ES and LS were conducted in 2016 and 2017,respectively.The mean temperatures during the filling stage were higher in ES,however,the daily temperatures at 7-10 days after flowering(DAF)in 2016,and at 5-10,13-14 DAF in 2017 were higher in LS.The results showed that amylose content in LS was lower than in ES with high amylose content rice varieties(HACV);the opposite trend occurred with low amylose content rice varieties(LACV).The mean starch granule diameter was higher in LS than ES in 2016,but the opposite result occurred in 2017 with all rice.Our results suggest that higher temperatures increased and decreased the amylose content in HACV and LACV,respectively.Temperatures at 5-15 DAF were important for the formation of starch granules:lower temperatures during 10-14 DAF increased the proportion of larger starch granules(d>6.21μm,some with d>13.3μm),and higher temperatures at 5-6 DAF increased the proportion of starch granules with diameter 4.24-6.21μm.

Research of Quality Standards for Stachydrine Hydrochloride in Chinese Medicine TJF Granule

A high-performance liquid chromatographic method was applied to the determination of stachydrine hydrochloride concentration in TJF granule (Chinese name: Tiao-Jing-Fang), using a mobile phase of methanol-acetonitrile (50:50, v/v) by the Agilent Kromasi NH2 column (250 mm × 4.6 mm, 5 μm, S/N: 22N25110). Detection wavelength was 201 nm. The result revealed good linearity of stachydrine hydrochloride and was obtained within the range of 0.20 - 1.98 μg/mL (R = 0.9995). The average recovery was 97.01%;the relative standard deviation (RSD) was 0.19%. To the best of our knowledge, this is the first report dedicated to the determination of stachydrine hydrochloride by the evaporative light scattering detector-high-performance liquid chromatographic (ELSD-HPLC) method.

Research Progress on Purification Process, Content Determination and Pharmacological Action of Atractylodin

Atractylodis Rhizoma comes from the dry rhizome of Atractylis lancea or Atractylodes chinensis in the Compositae family,and it is suitable for preventing and treating diseases such as cold,edema,night blindness and rheumatic arthralgia.Atractylodin is the main active component extracted and isolated from Atractylodis Rhizoma.A large number of studies have found that atractylodin has excellent drug activity in improving gastrointestinal emptying,anti-inflammation,inhibiting malignant tumor and reducing blood lipid.In this paper,the purification process and pharmacological activity of Atractylodin were summarized to provide a theoretical basis for basic research,clinical application and further development and utilization of atractylodin.

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.

Determination of Isoflavone from Soybean Lines Cultivated in Jilin Province and Correlation Analysis between Isoflavone Content and Soybean Quality

[Objective]The aim of this study was to set up a high performance liquid chromatography for rapid determination of isoflavones from soybean and analyze the correlation between isofalvone content and protein or fat content. [Method]The isoflavones were firstly extracted by 80% methanol and then hydrolyzed at 100 ℃. The chromatographic separation adopted a reversed-phase C18 analytical column with binary high-pressure gradient elution,while its analysis time was 25 min and column temperature was 40 ℃. The diode array detector was used for monitoring with wavelength of 260 nm. The correlation between isofalvone content and protein or fat content was analyzed by data processing system Origin 6.0. [Result]The high performance liquid chromatograph for determination of isoflavones from soybean was verified to be accurate and reliable by methodology. The isoflavones of 85 soybean lines cultivated in Jilin Province were determined,and the results primarily showed the characters and ranges of isoflavones from soybean lines cultivated in Jilin Province,while the isoflavone content of soybeans ranged from 2.29 to 4.89 mg/g,and the average content was 3.36 mg/g. The isoflavone content of 5 soybean lines exceeded 4 mg/g,while there was a remarkably negative correlation between isoflavone content and protein content,and there was no significant positive correlation between isoflavone content and fat content. [Conclusion]The isoflavone content of soybean lines cultivated in Jilin Province is higher,so it is feasible for breeding the soybean lines with high isoflavone content and fat contetnt.

Determination of Phytoene Content in Tomato Ketchup by HPLC

[Objective] The aim was to establish an HPLC method for determination of phytoene content in tomato ketchup. [Method] The chromatographic conditions were as follows： column, Agilent AT C18 （250 mm×4.6 mm, 5 μm）; mobile phase, methanol-THF （75：25）; detection wavelength, 287 nm; flow rate, 1.0 ml/min; column temperature, 30 ℃; sample size, 50 μl. [Result] There was a good linear relation- ship in the phytoene content range of 0.186-1.116μg. The average recovery rate was 103.8% with RSD of 1.47%. The phytoene content in the tomato ketchup sample was determined as 10.7 rag/100 g simple, accurate, rapid and reliable, and phytoene content in tomato ketchup. [Conclusion] The established method is it can be used for the determination of

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.

Determination of Coenzyme Q_(10) Content by RP-HPLC and Daily Change of Transmittance of Co-Q_(10)

[Objective] The aim of this study was to establish a reversed phase high-performance liquid chromatography（RP-HPLC）method for the content determination of Co-Q10.[Method] The RP-HPLC method was used to detect the Co-Q10,and the ultraviolet spectro-photometry was used to analyze the daily change of transmittance of Co-Q10.[Result] By using RP-HPLC,Co-Q10 had a good linear relationship between 40-300 μg/ml（r=0.999 9）.The limit of detection was 0.4 ng and the average recovery was 97.44%（n=3）.The system suitability of HP-HPLC was good,and the average recovery and precision results could meet the needs of assay.[Conclusion] This method was convenient,accurate and reproducible and could be used in quality control of Co-Q10.However,when it operates,light should be evaded.

Rapid Determination of Silicon Content in Rice

A method for rapid determination of silicon content in rice was introduced. The reliability of this method was verified by using a recombinant inbred line （RIL） population of rice cross Zhenshan 97B / Milyang 46. Two hundred and forty-nine RILs were transplanted in two replications. Simple correlation coefficients on the silicon content in the hull, flag leaf and stern in rice between duplicate samples of 498 rice materials were 0.97954, 0.97026 and 0.98848, respectively. Ten representative samples were selected for measurement using the high-temperature alkaline fusion method. Simple correlation coefficient between the silicon contents determined by the high-temperature alkaline fusion method and by the present method is 0.9993.

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.

Content Determination of Astragaloside Ⅳ in Astragalus from Three Different Regions by HPLC

[Objectives] The content of astragaloside in Astragalus membranaceus(Fisch.) Bge.var.mongholicus(Bge.) Hisao from three different regions was determined.[Methods] Referring to the method recorded in the Chinese Pharmacopoeia(2015 edition),the content of astragaloside IV in A.membranaceus was determined by HPLC.[Results] There were great differences in the astragaloside IV content of A.membranaceus among different regions.The content of astragaloside IV in A.membranaceus cultivated in Inner Mongolia was highest(0.155%),followed by that(0.143%) in A.membranaceus cultivated in Gansu,and the content of astragaloside IV in A.membranaceus cultivated in Shanxi was lowest(0.080%).The contents of astragaloside IV in A.membranaceus from different regions were all in line with the standard(not less than 0.040%) of Chinese Pharmacopoeia(2015 edition).[Conclusions]The content of astragaloside IV in A.membranaceus cultivated in three different regions met the medicinal standards.

Comparison between Double Crystals X-ray Diffraction and Micro-Raman Measurement on Composition Determination of High Ge Content Si_(1-x)Ge_(x) Layer Epitaxied on Si Substrate

It is important to acquire the composition of Si1-xGex layer, especially that with high Ge content, epitaxied on Si substrate. Two nondestructive examination methods, double crystals X-ray diffraction （DCXRD） and micro-Raman measurement, were introduced comparatively to determine x value in Si1-xGex layer, which show that while the two methods are consistent with each other when x is low, the results obtained from double crystals X-ray diffraction are not credible due to the large strain relaxation occurring in Si1-xGex layers when Ge content is higher than about 20%. Micro-Raman measurement is more appropriate for determining high Ge content than DCXRD.

Content Determination of Quercetin in Ferment of Ginkgo biloba L. Leaves by HPLC

[Objectives] This study aimed to determine the content of quercetin in ferment of Ginkgo biloba L.leaves.[Methods]Bacillus licheniformis was selected for solid-state fermentation of G.biloba leaf powder,and the content of quercetin in ferment of G.biloba leaves was determined by reversed-phase high-performance liquid chromatography.First,the flavonoid glycosides were extracted with methanol.Then,the flavonoid glycosides were hydrolyzed with hydrochloric acid to prepare the test solution.The chromatographic conditions were as follows:Platisil ODS C_(18) column(150 mm × 4.6 mm,5 μm);V_(methonal)∶V_(water)(0.4% phosphoric acid solution) =55∶45;flow rate of 1 m L/min;Shimadzu UV detector;detection wavelength of 360 nm.[Results] Quercetin was used as a reference substance.In the range of 0.002 6-0.036 0 g/L,there was a good linear relationship,with correlation coefficient of 0.999 8 and RSD of 1.26%.[Conclusions] This method is simple,easy to operate,accurate,and reproducible.It is suitable for the determination of quercetin content in G.biloba leaves.

Determination of Benzoylaconitine Compounds in the Decoctions of Aconiti Lateralis Radix Praeparata(Heishun Pieces),Trichosanthis Fructus and Their Combination

[Objectives]This study was conducted to determine the contents of benzoylmesaconine,benzoylaconitine and benzoylhypacoitine in the decoctions of Heishun pieces,Trichosanthis Fructus and their combination.[Methods]Heishun pieces,Trichosanthis Fructus and their combination were extracted for different time periods,and then grouped.HPLC was performed using an Agilent ZORBAX SB-C 18 chromatographic column(4.6 mm×250 mm,5μm)and acetonitrile-0.02 mol/L sodium dihydrogen phosphate as the mobile phase at a flow rate of 1 mL/min and a column temperature of 30℃,and the sample volume was 20μL.The detection wavelength was 230 nm.[Results]The total amounts of benzoylmesaconine,benzoylaconitine and benzoylhypacoitine in the single decoction group of Heishun pieces were all significantly different from those in the combined decoction group at corresponding time.[Conclusions]The total content of the benzoylaconitine type increased significantly after the combined decoction of Heishun pieces and Fructus Trichosanthis,which proves the scientificity of"eighteen incompatible medicaments,19 counteraction"in traditional Chinese medicine to some extent.

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.

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.