A novel multi-walled carbon nanotubes (MWCNTs) dispersive solid phase extraction (d-SPE) method which combined with gas chromatography (GC) coupled with electron capture detector (ECD) was developed for the determination of five pyrethroid pesticides in liquid milk for the first time. The effect of d-SPE conditions on the kinds of sorbent, MWCNTs and magnesium sulfate anhydro mass ratio, and extraction condition were researched, and then, the suitable method was found. Under the optimal conditions, the linear range was from 20 to 500 μg kg−1. The recoveries were from 81.8% to 112.1%, with the corresponding relative standard deviations (RSDs) less than 6%, correlation coefficients from 0.9978 to 0.9990, and limits of detection and quantification from 2.62 to 4.86 μg kg−1 and 8.73 to 16.2 μg kg−1. The proposed method is simple, fast, safe, and has high recovery and sensitivity applicable to analyze pyrethroid pesticides in liquid milk sample.
Authors:Y. Y. Di, Z. C. Tan, L. W. Li, S. L. Gao, and L. X. Sun
Low-temperature heat capacities of a solid complex Zn(Val)SO4·H2O(s) were measured by a precision automated adiabatic calorimeter over the temperature range between 78 and 373 K. The initial dehydration temperature of the coordination compound was determined to be, TD=327.05 K, by analysis of the heat-capacity curve. The experimental values of molar heat capacities were fitted to a polynomial equation of heat capacities (Cp,m) with the reduced temperatures (x), [x=f (T)], by least square method. The polynomial fitted values of the molar heat capacities and fundamental thermodynamic functions of the complex relative to the standard reference temperature 298.15 K were given with the interval of 5 K.
Enthalpies of dissolution of the [ZnSO4·7H2O(s)+Val(s)] (ΔsolHm,l0) and the Zn(Val)SO4·H2O(s) (ΔsolHm,20) in 100.00 mL of 2 mol dm−3 HCl(aq) at T=298.15 K were determined to be, ΔsolHm,l0=(94.588±0.025) kJ mol−1 and ΔsolHm,20=–(46.118±0.055) kJ mol−1, by means of a homemade isoperibol solution–reaction calorimeter. The standard molar enthalpy of formation of the compound was determined as: ΔfHm0 (Zn(Val)SO4·H2O(s), 298.15 K)=–(1850.97±1.92) kJ mol−1, from the enthalpies of dissolution and other auxiliary thermodynamic data through a Hess thermochemical cycle. Furthermore, the reliability of the Hess thermochemical cycle was verified by comparing UV/Vis spectra and the refractive indexes of solution A (from dissolution of the [ZnSO4·7H2O(s)+Val(s)] mixture in 2 mol dm−3 hydrochloric acid) and solution A’ (from dissolution of the complex Zn(Val)SO4·H2O(s) in 2 mol dm−3 hydrochloric acid).
The molar heat capacity Cp,m of 1,2-cyclohexane dicarboxylic anhydride was measured in the temperature range from T=80 to 390 K with a small sample automated adiabatic calorimeter. The melting point Tm, the molar enthalpy ΔfusHm and the entropy ΔfusSm of fusion for the compound were determined to be 303.80 K, 14.71 kJ mol−1 and 48.43 J K−1 mol−1, respectively. The thermodynamic functions [HT-H273.15] and [ST-S273.15] were derived in the temperature range from T=80 to 385 K with temperature interval of 5 K. The thermal stability of the compound was investigated by differential scanning
calorimeter (DSC) and thermogravimetry (TG), when the process of the mass-loss was due to the evaporation, instead of its
Authors:L. Ruan, Y. Liu, Z. Gao, P. Shen, and Q. Sheng
The thermogenic curves of the aerobic metabolism of the three strains of Bacillus thuringiensisB.t. A, B.t. B and B.t. C have been determined by using an LKB-2277 BioActivity Monitor. B.t. A was the host bacterium without foreign gene. B.t. B and B.t. C were constructed by transforming different foreign genes into the host B.t. A, respectively. B.t. B expressed erythromycin resistant gene, while B.t. C expressed both erythromycin resistant gene and tyrosinase gene. The heat flow rate of these strains is B.t. A> B.t. B >B.t. C. These results indicated that there is obvious interrelation between expression of foreign genes and heat flow rate of
Authors:W.Y. Gao, Y.W. Wang, L.M. Dong, and Z.W. Yu1
A microcalorimeter (Setaram c-80) was used
to study the thermokinetics of the hydration process of calcium phosphate
cement (CPC), a biocompatible biomaterial used in bone repair. The hydration
enthalpy was determined to be 35.8 J g–1
at 37.0°C when up to 80 mg CPC was dissolved in 2 mL of citric buffer.
In the present study, parameters related to time constants of the calorimeter
were obtained by fitting the recorded thermal curves with the function θ=Ae–?t(1– e–?2t).
The real thermogenetic curves were then retrieved with Tian function and the
transformation rate of the hydration process of CPC was found to follow the
The microstructures of the hydrated CPC were examined by scanning electron
microscopy. The nano-scale flake microstructures are due to crystallization
of calcium phosphate and they could contribute to the good biocompatibility
and high bioactivity.
Authors:Y. Zhang, X. An, X. Li, S. Chen, L. Gao, K. Wang, S. Wang, and Y. Yan
Two new y-type HMW-GSs in
with the mobility order of 1Dy12.2
>1Dy12, were identified by both SDS-PAGE and MALDI-TOF-MS. Molecular cloning and sequencing showed that the genes encoding subunits 1Dy12.1*
had identical nucleotide acid sequences with 1,947 bp encoding a mature protein of 627 residues. Their deduced molecular weights were 67,347.6 Da, satisfactorily corresponding to that of 1Dy12.2
subunit determined by MALDI-TOF-MS (67,015.7 Da), but was significantly smaller than that of the the 1Dy12.1*
subunit (68,577.1 Da). Both subunits showed high similarities to 1Dy10, suggesting that they could have a positive effect on bread-making quality. Interestingly, the expressed protein of the cloned ORF from accessions TD87 and TD130 in
co-migrated with subunit 1Dy12.2
, but moved slightly faster than 1Dy12.1*
on SDS-PAGE. The expressed protein in transgenic tobacco seeds, however, had the same mobility as the 1Dy12.1*
subunit, as confirmed by both SDS-PAGE and Western blotting. Although direct evidence of phosphoprotein could not be obtained by specific staining method, certain types of post-translational modifications (PTMs) of the 1Dy12.1*
subunit could not be excluded. We believe PTMs might be responsible for the molecular weight difference between the subunits 1Dy12.1*
Authors:L. N. Xu, F. Y. Gai, G. F. Mu, Y. Gao, H. T. Liu, and F. Luan
Formaldehyde in aquatic products was determined by micellar electrokinetic capillary chromatography (MEKC) after derivatization with 2,4-dinitrophenylhydrazine. Separation was carried out at 25 °C and 25 kV, using a fused silica capillary (75 µ internal diameter; 50.5 cm effective length) and an ultraviolet detector set at 360 nm. The optimal background electrolyte was 20 mM sodium tetraborate and 20 mM sodium dodecyl sulfate at pH 9.0 with 3 s hydrodynamic injection at 30 mbar. Electrophoretic analysis took approximately 6.5 min. The correlation coefficient of the calibration curve was 0.999 over the concentration range 2.0–100.0 mg L−1, and the LOD and LOQ values were 0.57 and 1.89 µg mL−1, respectively. The recoveries were from 83.7% to 97.2% with steam distillation as the sample pretreatment method.
Authors:G. Liu, L. Zhang, X. Qu, Y. Li, J. Gao, and L. Yang
A new model has been deduced by assumed autocatalytic reactions. It includes two rate constants, k1 and k2, two reaction orders, m and n, and the initial concentration of [OH]. The model proposed has been applied to the curing reaction of a system of bisphenol-S
epoxy resin (BPSER), with4,4'-diaminodiphenylmethane (DDM) as a curing agent. The curing reactions were studied by means of
differential scanning calorimetry (DSC). Analysis of DSC data indicated that an autocatalytic behavior showed in the curing
reaction. The new model was found to fit to the experimental data exactly. Rate constants, k1 and k2 were observed to be greater when curing temperature increased. The activation energies for k1 and k2 were 95.28 and 39.69 kJ mol–1, respectively. Diffusion control was incorporated to describe the cure in the latter stages.
Optimization of extraction ratio (ER) of tree peony seed protein (TPSP) was investigated using response surface methodology (RSM). The second-degree equation for ER of TPSP had high coeffi cient (0.9625) of determination. The probability (P) value of regression model signifi cance was less than 0.001 by analysis of central composite rotatable design. Relationships of ER to pH, liquid/solid ratio, squares of all factors, and cross-product factors (x2x3, x2x4, x3x4) were signifi cant (P<0.05). Whereas, extraction time, temperature, and cross-product terms (x1x2, x1x3, x1x4) were not signifi cant factors (P>0.05). Optimum extraction conditions were 3.42 h, pH 9.50, 50.80 ºC, and 9.54 ml g–1 of liquid/solid ratio with the maximum ER (43.60%) . SDS-PAGE indicated TPSP had mainly four proteins (180, 100, 60, and 35 kDa) with four subunits of 60, 48, 38, and 23 kDa. TPSP had a good amino acid composition with abundant essential amino acids (39.76%) determined by amino acid analysis.