薏苡仁油脂的化学成分分析

薏苡仁中提取的抗癌活性成分经药理筛选结果提示是中性油脂。为了确证油脂的化学成分，通过薄层层析法、气相层析及气－质分析，求得了薏苡仁甘油三酯的平均分子量为８７０．９７；明确了薏苡仁中性油脂的主要成分为甘油三酯（９１．４８±３．４３％）；脂肪酸残基为十六碳烷酸、十八碳烷酸、十八碳一烯酸、十八碳二烯酸；含酯量为９８０．６７±３．６９ｍｇ／ｇ，薏苡仁中性油脂的有效成分可通过含酯量的测定控制含量。

Comparison and Quality Assessment of Cassia Bark (Cortex Cinnamomi) by Thin Layer Chromatography

Aim To differentiate the genuine cassia bark from its substitutes and adulterants. Methods Six components, phenylpropyl acetate, cinnamyl acetate, cinnamaldehyde, cinnamyl alcohol, coumarin, and cinnamic acid were used as characteristic markers, and an optimized TLC method was developed. Results The TLC profile of cassia bark is similar to its closely related variety Cinnamomum cassia Presl var. macrophyllum Chu but significantly different from other six Cinnamomum species. High content of phenylpropyl acet...

Identification of Qishen Oral Solution with TLC and HPLC

[Objective] This study aimed to establish the standards for quality control of Qishen oral solution. [Method] Astragalus membranaceus, Atractylodes macro- cephala Koidz. and Glycyrrhiza uralensis in the preparation were identified by using thin layer chromatography （TLC）, and Codonopsis pilosula was identified by using high-performance liquid chromatography （HPLC）. [Result] By using the developed TLC system, experimental solution and reference solution showed clear spots, while negative control presented no interference. By using the developed HPLC system, the chromatographic peak of Iobetyolin was detected in experimental solution. [Con- clusion] The developed TLC and HPLC systems presented high specificity and good repeatability for identification of these four components and could be used in the quality control of Qishen oral solution.

Comparative Study of _(99m)TcN(NOEt)_2 and ^(99m)Tc-MIBI Imaging in Mice Bearing Ehrlich Ascites Tumor

Objective To evaluate and compare the ability to detect tumor by bis (N-ethoxy-N-ethyl dithiocarbamato) nitrido99mTc(V) [99mTcN(NOEt)2] and99mTc hexakis-2- methoxyisobutyl isonitrile [99mTc-MIBI]. Methods 99mTcN(NOEt)2 was prepared and quality control was performed using ascending thin-layer chromatography. Four mice bearing Ehrich ascites tumor cells underwent whole body planar imaging at 30 min, 2 h and 4 h after injection of99mTc-MIBI or99mTcN(NOEt)2. ROIs were drawn around the tumor, head, chest, and contralateral limbs in whole body planar images, and ratios of radioactivity in tumor in head (T/H), chest (T/C), and contralateral limbs (T/L) were calculated. The mice of99mTcN (NOEt)2 group were killed, then blood was collected, and the tumor and organs were excised, weighed and the radioactivity was measured. Results 99mTcN(NOEt)2 was stable after 4h at the room temperature.99mTcN(NOEt)2 was delivered to the tumor selectively and efficiently.99mTcN(NOEt)2 was found to provide excellent tumor-to-nontumor contrast for all the tissue except the abdomen. The T/L ratios increased to their maximums (4.87) at 2 h after injection. There was significant difference between the99mTcN(NOEt)2 imaging group and99mTc-MIBI imaging group. In vitro the radioactivity ratios per unit weight of tumor to blood, muscle, skeleton, lung, heart, and spleen were much higher than those of tumor to liver, instestine. Conclusion In mice bearing Ehrich ascites tumor,99mTcN(NOEt)2 exhibits a set of features essential for a good tracer for tumor imaging, including a rapid washout from blood, high uptake rate in tumor tissue, prolonged retention and high tumor-to-nontumor uptake ratio. The imaging quality of99mTcN(NOEt)2 was superior to that of99mTc-MIBI. These features indicate that99mTcN(NOEt)2 may be a better tracer to detect tumor than99mTc-MIBI. Key words tumor - radionuclide imaging - NOEt - MIBI

蜂蜜内掺入人工转化糖的检验

蜂蜜内掺假物之一是人工转化糖,它是由蔗糖(甜菜)用酸加热而制得,在水解时生成葡萄糖和果糖;同时有一部分果糖降解为羟甲基糖醛,并根据后者的验出可确认是掺入人工转化糖。俄学者阿加宁提出如下的色层谱法:(1)往瓷研钵内放入蜂蜜5—6g。

Determination of astaxanthin and astaxanthin esters in shrimp shell by HPLC

A method for determination of astaxanthin and astaxanthin eaters in shrimp shell by high performance liquid chromatography is established.Shrimp shell are addressed with 5%hydrochloric acid to remove calcium ions.After shell is dried,organics from shrimp shell are extracted with anhydrous ethanol.The alcohol extrative of the shrimp shell is mixed with the ammonium sulfate to extract astaxanthin by aqueous two-phase extraction.The crude astaxanthin is collected,which is distributed in the middle layer of the aqueous two-phase layer.After distilled water is added to the crude astaxanthin,the aqueous solution is centrifuged,and the previous step is repeated for several times.The precipitation in centrifuge tube is collected and dried.The crude astaxanthin dried is dissolved with acetone,and the sample solution is separated by TLC.Every pigment on the TLC plate is collected and dissolved with acetone.The pigments are determined by high performance liquid chromatograph.The results show that aqueous two-phase system,3 mL alcohol extractive of astaxanthin and 4.5 mL 20%ammonium sulfate,can be used to acquire crude astaxanthin.The wavelength of the maximum peak of astaxanthin in ethanol solution is 472 nm.A variety of pigments can be separated from the crude astaxanthin by thin-layer chromatography,including free astaxanthin,astaxanthin monoester,astaxanthin diester,echinenone and other substances.It can be seen from high performance liquid chromatography that the appearance time of free astaxanthin is from 4 min to 5.5 min,and the appearance time of astaxanthin monoester is from 10.5 min to 27.8 min.The method is simple about the sample pretreatment and feasible about the determination of astaxanthin and astaxanthin esters in shrimp shell.

Lipid and Fatty Acid Compositions of Cod (Gadus morhua),Haddock (Melanogrammus aeglefinus) and Halibut (Hippoglossus hippoglossus)

This study was conducted to compare lipid and fatty acid composition of cod,haddock and halibut.Three groups of cod（276 g±61 g）,haddock（538 g±83 g）and halibut（3704 g±221 g）were maintained with commercial feeds mainly based on fish meal and marine fish oil for 12 weeks prior to sampling.The fatty acid compositions of muscle and liver were determined by GC/FID after derivatization of extracted lipids into fatty acid methyl esters（FAME）.Lipids were also fractionated into neutral and polar lipids using Waters silica Sep-Pak（R）.The phospholipid fraction was further separated by high-performance thin-layer chromatography（HPTLC）and the FAME profile was obtained.Results of the present study showed that cod and haddock were lean fish and their total muscle lipid contents were 0.8% and 0.7%,respectively,with phospholipid constituting 83.6% and 87.5% of the total muscle lipid,respectively.Halibut was a medium-fat fish and its muscle lipid content was 8%,with 84% of the total muscle lipid being neutral lipid.Total liver lipid contents of cod,haddock and halibut were 36.9%,67.2% and 30.7%,respectively,of which the neutral lipids accounted for the major fraction（88.1%-97.1%）.Polyunsaturated fatty acids were the most abundant in cod and haddock muscle neutral lipid.Monounsaturated fatty acid level was the highest in halibut muscle neutral lipid.Fatty acid compositions of phospholipid were relatively constant.In summary,the liver of cod and haddock as lean fish was the main lipid reserve organ,and structural phospholipid is the major lipid form in flesh.However,as a medium-fat fish,halibut stored lipid in both their liver and muscle.

Isolation of Red Rose Anthocyanin Pigment and Its Application to Inhibit Lipid Oxidation in Yoghurt

Anthocyanin is a water soluble natural pigmen, which could be extracted from Red Rose. Color is an important factor to determine the quality of foods, so that the pigments isolation must be selected type of solvent for extraction process. Besides functioning as dyes, anthocyanins have a role as a good antioxidant, so it can be used to protect the fat content of fermented milk such as yoghurt. This experiment was to find out the effect of different solvent type on extraction pigment （aquadest： sitrat acid/lactic acid/sulfate acid/chloride acid） and to determine the effect of the addition of anthocyanins in protecting the fat content of yogurt on several levels addition. The research result showed that anthocyanin＇s pigment of red rose from petal flower＇s could be effective solvent extracted using lactic acid 0.02 M and increased fat stability of yoghurt. The anthocyanin pigment showed with HPLC analysis that pigment resulted TLC analysis at rite time 13.10 （as Cyanidin glucoside） and 22.61 （as Malvidin glucoside）. Yoghurt that given anthocyanin pigment has proven that fat content can be maintained its 86.7% （fat content with 2% pigment as such as 0.117% and without pigment 0.087%） after being stored for 6 days at cold and room temperature.

Fucoxanthin Content of Five Species Brown Seaweed from Talango District, Madura Island

Fucoxanthin content of five brown seaweed species of East Java collected from Talango district （Madura sea-Jawa sea） namely Padina australis, Turbinaria conoides, Sargassum cinereum, Sargassum filipendula and Sargassum echinocarpum were determined and samples were collected using Global Positioning System （GPS）. Fucoxanthin from those samples was determined using Thin Layer Chromatography （TLC）, High Pressure Liquid Chromatography （HPLC） and Spectrophotometer UV-Vis and the results were then calculated using Seely equation. The pigments separation using HPLC gave a better result compared to TLC, and beside fucoxanthin otlher pigments namely chlorophyll and β carotene were also identified in these samples. Four points of sampling location were chosen using GPS and spot with coordinate positions observed were 113.94444° EL-7.08795° SA; 113.94231° EL-7.08913° SA. The results showed that fucoxanthin content were as follow： Padina australis 0.2674± 0.0046 mg/g; Turbinaria conoides 0.2134± 0.0100 mg/g; Sargassum filipendula 0.1957 ± 0.0173 mg/g; Sargassum cinereum 0.1640 ± 0.0092 mg/g and Sargassum echinocarpum 0.1576 ± 0.0001 mg/g. It can be concluded that Padina australis and Turbinaria conoides contain the most amount of fucoxanthin and it is possible to be cultivated as edible brown seaweed fucoxanthin resources.

Production of Aflatoxins from Aspergillus flavus in Liquid Medium

Aflatoxins are produced mainly by Aspergillus flavus and Aspergillus parasiticus, and can be found in many grains such as peanuts, soybeans and com. This study aimed to qualitatively and quantitatively evaluate the production of aflatoxin in liquid media using strains of Aspergillus flavus obtained from peanuts marketed in the city of Fortaleza, CEo Strains of Aspergillus flavus were inoculated into a liquid medium malt extract and after 2 days inoculated into a second medium containing sucrose 5%, MgSO4·7H20 0.1%, KH2PO4 1%, ZnSO4·7H2O 0.0176 g, and cultured for 3 more days. The media were kept at room temperature ranging from 24°C to 32 °C with agitation of 130 rpm and aeration of 4.17 Llmin. Qualitative analysis was performed by thin layer chromatography and quantitatively by high performance liquid chromatography with fluorescence detection, demonstrating the production of aflatoxin B I （588 mg/L） and B2 （929 mg/L）.

Study on the Antioxidant Component of Fermented Rice Bran by Bacillus Natto

Each component of rice bran fermentation(RBF)of Bacillus natto was extracted and its antioxidant activity was tested.By dint of thin layer chromatography,the antioxidant components were separated.The sample isolated from TLC for ethyl acetate phase and ether phase was analyzed by GC-MS.Results indicated that the antioxidant activity of large components in rice bran fermentation was low.The constituents of extracted phase had antioxidant activity apart from the petroleum ether phase.The constituents of ethyl acetate phase and Ether phase had best antioxidant activity,163 and 168 kU/g,respectively.The main composition of ethyl acetate phase was allyl group methyl-thioether and the main composition of ether phase included 3,5-dimethyl phenol,2,4-dipl-tert-Butyl and Fluazifop.

Qualitative and Quantitative Analysis of Linoleic Acid in Polygonati Rhizoma

Objective To explore the major compound in Polygonati Rhizoma(Huang Jing,黄精)for quality control.Methods The major compound was isolated and analyzed by liquid chromatography-mass spectrometry(LC-MS),and subsequently further identified by nuclear magnetic resonance(NMR).Thin layer chromatography(TLC)was optimized based on the previous methods reported in the Chinese Pharmacopeia(2015 edition).Results The major compound was isolated from the natural material and identified as linoleic acid.A high performance liquid chromatography(HPLC)method with robust linearity(R2=0.9997),specificity,precision,stability,repeatability and recovery was developed for linoleic acid determination.TLC chromatogram was improved significantly after optimization for qualitative analysis.Conclusions The optimized TLC method is practical and can be adopted for quality control of Polygonati Rhizoma(Huang Jing,黄精).The levels of linoleic acid vary between species of Polygonati Rhizoma(Huang Jing,黄精),with Polygonatum cyrtonema Hua(Jiang Xing Huang Jing,姜型黄精)showing the highest contents.This study provides valuable information for quality control of Polygonati Rhizoma(Huang Jing,黄精).

Colorimetric Method for Determination of Amino Acids on Thin Layer and Filter Paper Chromatography Using a Modified Ninhydrin Reagent

A simple and rapid colorimetric method for the and Whatman filter paper chromatography is described. determination of some amino acids on thin layer chromatography （TLC） The studied compounds are cysteine, proline, methionine, tryptophan glutmine, glycine, thyrosine, threonine, leucine and lysine. The method is based on the formation of color from the reaction of stannous chloride （SnCI2） and ninhydrin reagents. The procedure has been successfully applied to the assay of the standard amino acid preparation after TLC separation, and the results of the studied compounds were clear and favorable, comparing to the official methods. However, the improved TLC is much more efficient for the detection of amino acid. The main advantage of this method is that the detection of amino acids can be preformed visually.

Biodiesel synthesis via metal oxides and metal chlorides catalysis from marine alga Melanothamnus afaqhusainii

This research article demonstrates the most comprehensive comparative catalytic study of different metal oxides and metal chlorides towards the methanolysis of triglycerides of marine red macroalga Melanothamnus alhqhusainii. CaO was found to be the most reactive metal oxide that yielded 80% biodiesel while ZnCI2 was the most reactive metal chloride that produced 60% biodiesel by mechanical stirring for 6 h at 100-110 ℃. The overall reactivity order of the catalysts was found to be CaO 〉 MgO 〉 Pb02 〉 ZnC12 〉 TIC14 〉 PbO 〉 HgC12 〉 ZnO 〉 AIC13 〉 SnCI2 〉 TiO2 whereas, CaCI2, MgCI2, A1203, HgO, PbCI2, MnO2, MnC12, Fe203 and FeCI3 were found to be non-reactive for transesterification of triglycerides. In addition, a detailed study of the screening of mobile phases and spraying reagents was conducted which showed that petroleum ether ： chloroform ： toluene （7：2：1 ） is the best mobile phase, whereas iodine crystals/silica gel is the best visualizing agent for the thin layer chroma- tography （TLC） examination ofbiodiesel. Biodiesel production was confirmed by comparative TLC examination. It was further supported by the determination of fuel properties of biodiesel, which were found to be similar to the standard limits of American Society for Testing and Materials （ASTM）,

Preparation, Characterization and Biological Activity Studies of New Azo Compounds

A new series of azo were derived from 2,5-di（p-amino phenyl）-3,6-diphenyl pyrazine in the presence of benzoic acid, salicylic acid, p-amino salicylic acid, p-methoxy phenol and pmethyl phenol. The structures of the synthesized compounds were determined on the basis of their FTIR, UV （ultraviolet）, elemental analysis and H-NMR （H-nuclear magnetic resonance） spectral date. The purity of synthesized compounds was checked by performing TLC （thin layer chromatography）. The antibacterial activity was evaluated in DMSO （dimethyl sulfoxide）.

Optimization of Isolation and Identification Conditions of Glibenclamide Annotation

A method for dispersive liquid-liquid microextraction of glibenclamide on model mixtures with urine has been developed. The extraction conditions have been optimized and the influence of extractants and dispersing agent for allocation of toxicant from biosubstrate has been experimentally established. The method of TLC （thin layer chromatography） screening in order to remove endogenous and exogenous substances has been developed. The method of IR-spectroscopy for confirmatory analysis has been used. The combination of the two methods of analysis allows identifying glibenclamide quickly and reliably isolated from bioliquid and reducing the risk of false-positive results.

Bioequivalence of Two Brands of Valsartan 80 mg Coated Breakable Tablets in 15 Healthy Algerian Volunteers： A Pilot Study

A randomized, two-way, crossover study was conducted in 15 fasting, healthy, Algerian volunteers to compare the bioavailability of two brands of Valsartan 80 mg coated breakable tablets. The present study aimed to evaluate the intra-subject variability of this active substance in the Algerian population. The test brand was compared to TAREG （Novartis） as the reference product. The study was performed at the bioequivalence center of the national control laboratory for pharmaceuticals products, in joint venture with University Hospital Center Ibn Badis, Constantine, Algeria. The drug was administered with 200 mL of water after a 10 h overnight fasting on two treatment days separated by one week washout period. After dosing, serial blood samples were collected for a period of 24 h. A reliable, simple, and robust liquid chromatography-tandem mass spectro-metric （LC-MS/MS） method has been developed and validated that employs protein precipitation （or denaturation） for the estimation of valsartan in human plasma using losartan as internal standard. The assay was found to be linear over the range of 50-5,000 ng/mL, with a lower limit of quantitation of 50ng/mL. Various pharnaacokinetic parameters including AUC0-t, AUC∞, Cmax, Tmax, and TI/2 were determined from plasma concentrations of both formulations and found to be in good agreement with reported values. The pharmacokinetical and statistical analysis was conducted with Kinetica 4.4.1. AUC0.t, AUC0-∞ and Cmax were tested for bioequivalence after log-transformation of data. No significant difference was found based on ANOVA; 90% confidence interval （[85.82%, 118.76%] for AUC0.t [86.09%, 118.83%] for AUC0-∞） of test/reference ratio for these parameters were found within bioequivalence acceptance range of 80-125%. But for the Cmax, the 90% confidence interval of test/reference ratio wasn＇t in this acceptance range [90.18%, 131.07%] .The results of PK analysis suggested that the reference and test formulations ofvalsartan 80 mg coated breakable tablets weren＇t bioequivalent during fasting state in these healthy algerian volunteers.

Ethanol-Water Near-Azeotropic Mixture Dehydration by Compound Starch-Based Adsorbent

Ethanol-water near-azeotropic mixture dehydration was investigated by formulated compound starchbased adsorbent(CSA), which consists of corn, sweet potato and foaming agent. The net retention time and separation factor of water over ethanol were measured by inverse gas chromatography(IGC). Results indicated that water has a longer net retention time than ethanol and that low temperature is beneficial to this dehydration process. Orthogonal test was conducted under different vapor feed flow rates, bed temperatures and bed heights, to obtain optimal fixed-bed dehydration condition. Dynamic saturated adsorbance was also studied. It was found that CSA has the same water adsorption capacity(0.15 g/g)as some commercial molecular sieves. Besides, this biosorptive dehydration process was found to be the most energy-efficient compared with other ethanol purification processes.

Establishing a Quality Control System of Hedyotis corymbosa

Objective Hedyotis corymbosa(Shui Xian Cao,水线草,HC)is the main antitumor medicine in China and other southeast Asian countries.A comprehensive quality control system of HC was established in this study,as the current system was ineffective.Methods Microscopy was used to observe the characteristics of the powder and cross-sectional tissue.Thin layer chromatography(TLC)was employed to separate HC from Hedyotis diffusa(Bai Hua She She Cao,白花蛇舌草,HD).Simultaneously,high-performance liquid chromatography(HPLC)was used to establish the characteristic spectrum of HC and determine the concentrations of hedyotiscone A.Regarding the issue of systematicness,concentrations of water,total ash,acid-insoluble ash,heavy metals(including lead,arsenic,mercury,cadmium and copper)and pesticide residue were measured by the methods described in the 2015 edition of Chinese Pharmacopoeia.Results Calcium oxalate needle crystal bundles and oil drops were observed in the cross-sectional tissue.Three characteristic blue fluorescent spots were observed in the HC samples by TLC.There were five distinct characteristic peaks in HC but not in HD,and hedyotiscone A was the sharpest characteristic peak.The generated linear equation of hedyotiscone A was Y=3.15×108X+312.04(r2=1.000)between 0.00005270 and 0.002108 mg/mL,and the average recovery was 100.42%.Precision[relative standard deviation(RSD)0.92%],repeatability(RSD 0.14%),and recovery(RSD 0.85%)met the requirements for quantitative analysis.Hedyotiscone A concentrations ranged from 0.00017%~0.00113%across different habitats.Concentrations of water,ash and acid-insoluble ash were 8.80%~11.2%,7.00%~15.3%and 0.440%~7.70%,respectively.Concentrations of Pb,As,Hg,Cd and Cu were 1.60~4.60,0.650~1.60,0.0300~0.100,0.240~0.690 and 10.1~16.6μg/g,respectively.Pesticide residues were less than 0.00100 ppm.Conclusion The quality control system can effectively distinguish HC from HD,so as to comprehensively control the quality of HC,to provide references for the clinical use of HC.

Seasonal variations of carboxylic acids and their contributions to the rainwater acidity: A case study of Guiyang and Shangzhong,China

Low molecule weight carboxylic acids are ubiquitous and important chemical constituents in the troposphere.Seven carboxylic acids in the rainwater of Guiyang and Shangzhong were simultaneously determined by ion chromatography from April 2006 to April 2007.Formic, acetic and oxalic acids were found to be the predominant carboxylic acids.Their volume weighted average concentration (VWA) in the rainwater of Guiyang were 14.24 μmol/L, 9.35 μmol/L and 2.79 μmol/L, respectively;as compared to 4.95 μmol/L, 1.35 μmol/L and 2.31 μmol/L in the rainwater of Shangzhong.In Shangzhong it is witnessed that the concentra-tions of these acids were higher in the summer than in the winter and direct emissions from vegetations or soils may account for the main provenance of the acids.This is, however, not the case in Guiyang, where the concentrations of the carboxylic acids were higher during the non-growing season than during the growing season.The relatively weak scavenging affected by scarce and little rainwater as well as the particles accompanied with the rainfall may have some effect on the carboxylic acids during the wintertime in Guiyang.Carboxylic acids in the rainwater of Guiyang were estimated to account for 18.7% to the free acidity, where formic, acetic and oxalic acids accounted for 7.9%, 4.7%, 6.1%, respectively.In Shangzhong, the 3 primary carboxylic acids represented 58.1% to the free acidity where formic, acetic and oxalic acids represented 25.1%, 7.5%, 25.5%, respectively.Carboxylic anions accounted for 6.6% (1.7%–19.2%) to the total anions in the rainwater of Guiyang.Carboxylic anions repre-sented 13.2% (0.5%–92.2%) to the total anions in the rainwater of Shangzhong.These results indicated that carboxylic acids were the important contributors to the rainwater acidity, especially in remote regions.