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.

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.

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.

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.

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.

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.

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.

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 ...

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.

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.

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.

Preparation and Characterization of the Phenolated Wood Using Sulfuric Acid as a Catalyst Ⅱ. FT-IR and GPC Characterization

By means of gel permeation chromatography analysis, the molecular weight of liquefied wood under different reaction conditions was investigated to trace the change in the structural characteristics of the liquefied wood. The insoluble residues were analyzed by Fourier transform infrared to investigate the liquefaction order of three main wood components. The results indicate that both reaction temperature and reaction time could affect the molecular characteristics of the liquefied wood obtained. The mo...

COPPER(0)-MEDIATED RADICAL POLYMERIZATION OF STYRENE AT ROOM TEMPERATURE

The ＂living＇/controlled radical polymerization （LRP） of styrene （St） at room temperature is rarely reported. In this work, copper（0） （Cu（0））-mediated radical polymerization of St at room temperature was investigated in detail. Dimethyl sulfoxide （DMSO）, N,N-dimethylformamide （DMF） as well as a binary solvent, tetrahydrofuravdl,l,l,3,3,3-hexafluoro-2- propanol were used as the solvents, respectively. Methyl-2-bromopropionate and ethyl 2-bromoisobutyrate were used as the initiators, respectively. The polymerization proceeded smoothly with moderate conversions at room temperature. It was found that DMF was a good solvent with the essential features of LRP, while DMSO was a poor solvent with uncontrollable molecular weights. Besides, the match among the initiator, solvent and molar ratios of reactants can modulate the livingness of the polymerization, and the proper selection of ligand was also crucial to a controlled process. This work provided a first example of Cu（0）-mediated radical polymerization of St at room temperature, which would enrich and strength the LRP technique.