Determination of 14 Organophosphorus Pesticide Residues in Mutton by Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry(GPC-GC-MS)

[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry(GC-MS)in selective ion scanning mode(SIM).[Results]The organophosphorus pesticide standard solutions showed good linearity in the mass concentration range of 0.1-10.0μg/ml with correlation coefficients(r)not lower than 0.999,and the detection limits(S=3 N)ranged from 0.01 to 0.05 mg/kg.The average recovery values were in the range of 80.2%-99.7%,with relative standard deviations(RSDs,n=3)in the range of 1.8%-6.3%,at the addition levels of 0.5,1.0 and 2.0 mg/kg.[Conclusions]The method is simple,sensitive and accurate,and can be used for the determination of organophosphorus pesticide residues in mutton.

Gel Filtration Chromatography Combined with Bradford Method for Determination of Total Residual Protein in Ferment Antibiotics

Aim A novel method has been developed for evaluation of the levels of total residual protein in antibiotics produced by fermentation using gel filtration chromatography (GFC) combined with Bradford assay based on determination of residual protein in lincomycin hydrochloride. Methods The chromatographic conditions were SuperdexTM peptide column, 0.01 mol*L-1 phosphate buffer solution as mobile phase, and flow rate of 1 mL·min-1. Five hundred microliters of lincomycin hydrochloride solution (3 g of lincomycin hydrochloride dissolved in 10 mL of mobile phase) was injected into the chromatograph and the eluted solution was collected between 6 min and 14.5 min (protein eluted from column within this period), and the residual content of total protein in the eluted solution was assayed using Bradford assay method. Results The average recovery was more than 90% for bovine serum albumin, the calibration equation for the range of 0-12 μg·mL-1 of protein was y=-0.002 4x2+0.064 2x+0.002 9, r2=0.999 9, RSD=0.1%-0.9%, and the LOD and LOQ were 3 and 10 ng·mL-1 of protein, respectively. Conclusion The novel method for determining the residual protein in ferment antibio-tics is simple, rapid, and precise.

Determination of Steroid Hormone Residues in Fish Tissues Using Gel Permeation Chromatography and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L^(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg^(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg^(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues.

Separation and purification of deoxynivalenol(DON) mycotoxin from wheat culture using a simple two-step silica gel column chromatography

Deoxynivalenol（DON） is a type B trichothecenes mycotoxin produced by several Fusarium species, often found in foodstuffs for humans and animals. DON is in great demand for the toxicological researches both in vivo and in vitro. In this work, wheat culture was inoculated with a Fusarium graminearum PH-1 strain for DON production. The solvent system for crude extraction was acetonitrile-water（84：16, v/v）. A simple two-step silica gel column chromatography was employed to separate the DON mycotoxin from wheat culture, combined with preparative high performance liquid chromatography（preparative HPLC） to purify the compound. The solvent system for the second silica gel column chromatography was methylene chloride-methanol（17：1, v/v）, which provided a good elution effect selected on thin layer chromatography（TLC）. The target compound was identified by HPLC, and the chemical structure was confirmed by mass spectrometry（MS） and ~1H and ^（13）C nuclear magnetic resonance（NMR） spectroscopy. A total of 433 mg of purified DON was obtained from 1 kg of wheat culture, with a purity of 99.01%. The study had provided an easy-operating and cost-effective method to isolate an expensive compound in a simple way.

GEL PERMEATION CHROMATOGRAPHIC ANALYSIS OF LACQUER POLYSACCHARIDE

Ten fractionated samples of Chinese lacquer polysaccharide in aqueous 0.1M NaC1 solution were studied by aqueous-phase gel permeation chromatography （GPC）. The universal calibration, broad MWD calibration and corrected column dispersion were adopted to the analysis of GPC chromatograms of the polysaccharide. The molecular weights M;, M;and polydispersity index M;/M;obtained from GPC are in good agreement with the results of light scattering and membrane osmometry. It is verified that the universal calibration concept is applicable to the lacquer polysaccharide having a number of side chains.

Thermal aging behavior of high performance poly(vinyl alcohol) hydrogel

The thermal aging behavior of poly （ vinyl alcohol ） （ PVA ） hydrogel was studied at four different temperatures of 40 ℃, 50 ℃, 60 ℃ and 70 ℃ in one year. The samples of PVA hydrogel were closely covered by plastic film. The changes of their chemical structures and physical properties during aging were measured through different measurable techniques including tensile testing, gel permeation chromatography （ GPC ）, viscosity analysis, and Fourier transform infrared （FTIR） spec- trum. The results showed that the molecular weight of PVA in hydrogel changed little with time and temperature. FTIR spectra of PVA in all the samples were similar to those of the original samples. The tensile strength of PVA hydrogel didn＇t change until the 330th days.

The effect of reactive plasticizer on viscoelastic and mechanical properties of solid rocket propellants based on different types of HTPB resin

Conventional plasticizers deteriorate mechanical and viscoelastic properties of the propellants due to their migration upon aging and long-term storage,which affects reliability and safety properties during exploitation.To address this issue,conventional plasticizer,dioctyl adipate(DOA),is replaced by reactive one,castor oil(CO).In addition,three different types of HTPB were used to obtain propellants with designed viscoelastic and mechanical properties.The CO increased propellants viscosity,without a significant impact on the propellant processability,regardless to the type of prepolymer.Conversely,mechanical properties were different depending on the type of resin,which were further analyzed by gel permeation chromatography(GPC).Addition of CO formed a denser polymer network and shifted T_(g) to higher values,compared to the compositions with DOA.The tensile strength of CO-containing propellants was lower at +20℃ and +50℃ compared to the reference compositions,while the strain at maximum load and strain at break were significantly increased with pronounced plastic deformation,especially for samples at -30℃.The inclusion of CO in the propellants composition gives more room for adjusting a wide range of mechanical properties.

凝胶渗透色谱和气相色谱-质谱法测定动物食品中27种有机氯和15种拟除虫菊酯类农药残留量

A GC-MS method for the determination of 27 organochlorine pesticides and 15 Pyrethroid pesticides in animal food is established.The method was based on Gel Permeation chromatography combined with solid-phase extraction for sample preparation.Rapid qualitative and quantitative analyses was carried out by gas chromatography-mass spectrometry under the selective-ion monitoring mode.The experimental results showed that the correlation coefficients were better than 0.99,the recoveries for spiked standards were 70%-104%,the relative standard deviations were 2.1%-15.9%.

Study on ternary polymerization of toluene diisocyanate

For the production of reactive polyurethane cross-linkinger and curing agents, 2, 4-diisocyanate toluene （TDI） terpolymer, which possesses the rigid structures of hexatomic ring and three reactive functional groups, was synthesized and characterized by the Fourier transform infrared （FFIR）, the gel permeation chromatography （GPC） and the chemical analysis methods. The reaction conditions were studied and optimized. A tracking research on the polymerization process of TDI was taken by using the GPC. The formation processes of the terpolymer, oligomers and higher-polymers were also dealt with. Results show that the TDI terpolymer can be prepared in the presence of Cat-3 catalyst and at the reaction temperature of （60 ±2）℃. The reaction time is short, its outcomes have narrow molecular weights distribution, namely molecular weights from 530 to 550, Mw/Mn =1.10, and the mass fraction of NCO is （25. 0 ± 0. 5）%. With the reaction time prolonging, however, TDI can be further higher-polymedzed to form higher-polymers. Benzoyl chloride （0. 4%, mass fraction）, as the stabilizing agent, can effectively inhibit the occurrence of higher-polymerization. The obtained TDI terpolymer can be stable for more than half a year.

Isolation and Purification of Gonyautoxins from Two Strain of Alexandrium minutum Halim

Aim To study isolation and purification of Gonyautoxins from two differentstrains of Alexandrium minutum Halim. Methods Ethanol extracts of the two culture strains ofAlexandrium minutum Halim were fractionated by gel filtration and ion exchange chromatography toobtain gonyautoxins. The toxin profiles were tested by HPLC method. Results Both strains containgonyautoxin-1, gonyautoxin-2, gonyautoxin-3 and gonyautoxin-4. The total gonyautoxin content ofAmtk4 strain is almost 10 times higher than that of Amtk2 strain. Conclusion Alexandrium minutumHalim Amtk4 strain is suitable for the preparation of Gonyautoxins.

Characterization of Crude Cellulase from Trichoderma reesei and Purification of Cellulase

The gel filtration was carried out for purification of cellulase. The influences of chromatographic parameters on the resolution were studied to determine the optimal conditions for purification. The purified endoglucanase was obtained by gel filtration by Superdex 75 prep grade with an activity recovery of 92.8% and the purification factor 4.2. The sample volume should be below 6% of the column bed volume and the column bed height L≥12.0 cm. The optimum catalysis temperature and pH for the enzyme were 55 ℃ and 4.5—5.0, respectively. The cellulase was stable at pH ranging from 4.0 to 6.0 and temperature below 60 ℃.

Discrimination of Car Headlight Plastic by Gel Permeation Chromatography

Car headlight plastic as a kind of evidence often can be seen in traffic accidents and some other cases.We tested 20 brands of car headlight plastic using gel chromatography.The data were processed using the Statistical Package for the Social Sciences(SPSS)one‑way analysis of variance(ANOVA)and the discrimination rate was 97.14%.This indicated that we could discriminate between different headlights by the molecular weight of their headlight plastic.Gel permeation chromatography is an effective method of discriminating between headlights,particularly in the case of a traffic accident.

Recombinant human bone morphogenetic protein-7 expressed from CHO cells possessing the activity of bone-induced in vitro

Objective To express the recombinant human bone morphogenetic protein-7 (rhBMP-7) in Chinese hamster ovary (CHO) cells and to establish the in vitro biological activity assay of rhBMP-7. Methods Human BMP-7 cDNA was subcloned into pcDNA3.1 mammalian expression vector and transfected to CHO cells by using the lipofectin transfection method. BMP-7 expression cell culture supernatants were harvested and purified for target protein. To analyze the bioactivity of the secreted rhBMP-7, a novel in vitro assay was established by measuring its alkaline phosphatase (ALP) stimulating of osteoblast cell line, W-20-17. Results BMP-7 stably expressing cell clone was selected, which secreted mature disulfide-linked homodimer form of hBMP-7 and had an apparent molecular weight of 36kDa. rhBMP-7 with >95% purity was obtained using 3 step chromatography method. Bioactivity assay showed that the purified protein specifically stimulated W-20-17 cell producing ALP, with a 4-fold increase of ALP activity at 100ng/ml or more, and the EC50 of 15.6ng/ml. Conclusion Purified rhBMP-7 from this CHO expression system has significant biological activity in induction of osteoblast phenotype, which demonstrates potential bone regeneration activity.

Optimization of Extraction Methods of ROP GTPase from Young Leaves of Wheat

All of the Rho GTPase seems to form a special sub-family,because such a sub-family has so far only found in plants,and then named Rop GTPase,which directly involved in and regulated of muscle actin cytoskeletal reorganization,such as a series of signal transductions.The efficient purification technology and the means of ROP GTPase in wheat are the key basis of the studies on its functions and prosperities.And it has a very important theoretical and practical significance in the signal transduction and F-act...

Epithermal Ageing Mechanism of Gussasphalt

The normal asphalt index test, DSR test, FTIR and the GPC distribution analysis of molecular weight on the extraction and recovery of asphalt of the gussasphalt, SMA extraction and recovery of asphalt and the rotary-thin-film-oven-aged asphalt above 240 ℃ were introduced. The results indicate the rutting factor and fatigue factor of the extraction and recovery of asphalt of the gussasphalt are greatly improved, and an obvious absorption peak of carbonyl and a further decrease of the SBS molecular weight of the gussasphalt are found.

Fractionation of edible bird’s nest glycoprotein hydrolysates:characterisation and antioxidative activities of the fractions

E dible bird’s nest(EBN)hydrolysates have been proven to exhibit enhanced bioactivities.However,being a macromolecule,fractions with different molecular weights would have different properties and bioactivities.Hence,this research was aimed to determine the chemical properties and antioxidant activities of freezedried(EBN_(FD))and spray-dried EBN(EBN_(SD))hydrolysates fractionated using gel permeation chromatography(GPC).Overall,two well-separated fractions were identified(EBN_(fFD1),EBN_(fFD2),EBN_(fSD1) and EBN_(fSD2)).EBNFD demonstrated significantly higher(P≤0.05)peptide(3.6%),total carbohydrate(27.7%)and sialic acid(18.2%)contents than that of EBNSD.Similar trend was observed in low molecular weight fractionates(EBN_(fFD2) and EBN_(fSD2)).Meanwhile,the first fractionates(EBN_(fFD1) and EBN_(fSD1))exhibited significantly higher(P≤0.05)hydroxyl radical(·OH)scavenging activity.Fourier transform infrared(FTIR)spectroscopy demonstrated that all EBN fractionates have similar spectrum,except in the region of N—H(amideⅡ)and C—H alkyl group.In conclusion,EBN fractionates with different molecular weights showed different chemical properties and antioxidant activities.

Characterization of self-assembled nano-phase silane-based particle coating

Self-assembled nano-phase silane-based particle coating was prepared through sol-gel technique.Tetramethoxysilane and 3-glycidoxypropyltrimethoxysilane were used as precursors for the self-assembled sol-gel coatings.The silane colloidal particle size was analyzed by laser particle size measurement.The results indicate that the particle size is in nano-scale and the diameter of particles deceases with increasing dilution times.Gel permeation chromatography proves that the relative molecular mass of macromolecule in a referenced sol solution is 1220-1240 amu.A simulation model was proposed to study the siloxane structure.Fourier transform infrared spectra of solution and film prove the disappearing of epoxy bond.The results of solid-state 13C and 29Si nuclear magnetic resonance experiments indicate the formation of Si-O-Si network.Potentiodynamic analysis shows that the self-assembled coating has excellent corrosion resistance.Salt fog tests prove that 2-methyl piperidine as inhibitor significantly improves the corrosion resistance of the self-assembled coating.

Fractionation of gamma-glutamyltransferase in patients with nonalcoholic fatty liver disease and alcoholic liver disease

AIM To assess how serum gamma-glutamyltransferase(GGT) fractions vary in patients with alcoholic liver disease(ALD) and non-alcoholic fatty liver disease(NAFLD). METHODS Serum samples were obtained from 14 patients with biopsy-proven alcoholic liver diseases and 9 patients with biopsy proven non-alcoholic fatty liver disease. In addition to these biopsy-proven cases, 16 obese(body mass index > 25) patients without any history of alcohol consumption but with a fatty liver on ultrasound examination and with elevated GGT were included for an additional analysis. Serum GGT fractionation was conducted by high-performance gel filtration liquid chromatography and was separated into the four fractions, big-GGT, medium-GGT, small-GGT(s-GGT), and free-GGT(f-GGT).RESULTS The results were expressed as a ratio of each fraction including the total GGT(t-GGT). The s-GGT/t-GGT ratioswere lowest for the control group and highest for the ALD group. The differences between the control and NAFLD groups and also between the NAFLD and ALD groups were statistically significant. In contrast, the f-GGT/t-GGT ratios were highest in the control group and lowest in the ALD group, with the differences being statistically significant. As a result, the s-GGT/f-GGT ratios were markedly increased in the NAFLD group as compared with the control group. The increase of the s-GGT/t-GGT ratios, the decrease of the f-GGT/t-GGT ratios, and the increase of s-GGT/F-GGT ratios as compared with the control group subjects were also found in obese patients with clinically diagnosed fatty change of the liver.CONCLUSION Serum GGT fractionation by high-performance gel filtration liquid chromatography is potentially useful for the differential diagnosis of ALD and NAFLD.

SUPPORTED ZIEGLER-NATTA CATALYSTS FOR ETHYLENE SLURRY POLYMERIZATION AND CONTROL OF MOLECULAR WEIGHT DISTRIBUTION OF POLYETHYLENE

The effect of chemical composition of highly active supported Ziegler-Natta catalysts with controlled morphology on the MWD of PE has been studied.It was shown the variation of transition metal compound in the MgCl_2-supported catalyst affect of MWD of PE produced in broad range:Vanadium-magnesium catalyst(VMC)produce PE with broad and bimodal MWD(M_w/M_n=14-21).MWD of PE,produced over titanium-magnesium catalyst(TMC)is narrow or medium depending on Ti content in the catalyst(M_w/M_n=3.1-4.8).The oxidation ...

LIGHT SCATTERING OF POLYSACCHARIDE FROM LACQUER IN AQUEOUS SOLUTION

The polysaccharide having weight-average molecular weight M_w=1. 09×10~5, isolated from the sap of lac trees (Vietnam), was separated into 12 fractions by aqueous-phase preparative gel permeation chromatography. The molecular weights and molecular weight distributions of the fractions were measured in aqueous 0.08M KCl/0.01 M NaAc and 0.4M KCl/0.05M NaAc at pH =7. 6 by light scattering, viscometry and gel permeation chromatography. The Mark-Houwink equation in aqueous 0.08M KCl/0.01M NaAc at 30℃ was found to be [η]= 2.28×10^(-2) M_w^(0.52) (cm^3/g), which indicated the polysaccharide chain in the aqueous solution to be a spherical random coil.