Determination of histamine in tomatoes by liquid chromatography/mass spectrometry

The histamine level in tomato fruits and pastes was determined by 2 orthogonal techniques as a means of comparing accuracy. Close statistical agreement was found between assays for free histamine by capillary electrophoresis (with UV absorbance detection), and for the dansyl derivative by reversed-phase liquid chromatography (LC). Both techniques have adequate sensitivity for the analysis of endogenous histamine in tomatoes, but LC/electrospray tandem mass spectrometry was more sensitive by at least an order of magnitude, down to a level of 0.05 mg/kg.     

The influence of monomer chemistry on radical formation and secondary reactions during electron-beam polymerization

The vast majority of industrial electron-beam (EB) polymerizations are initiated via radical mechanism. Because radicals drive EB polymerization, understanding their formation and secondary reactions can provide insight into polymerization kinetics and property development. Primary and initiating radicals were quantified by measuring G(R^•) and G(M^•) , respectively, for various acrylate and methacrylate monomers. Monomer chemistry was shown to impact primary radical formation; however, increased primary radical concentration did not necessarily correlate to increased conversion. Despite exhibiting high values of G(R^•) , methacrylates achieved very little conversion and had G(M^•) values near zero. Acrylates achieved much higher G(M^•) values and rates of polymerization compared to their methacrylate counterparts. Additionally, the efficiency of primary radicals converting to initiating radicals, f(M^•) , for each acrylate monomer was shown to be a good predictor of the amount of gel fraction formed during polymerization. Understanding radical formation and secondary radical reactions can help guide the structure/processing conditions/properties relationships that are currently underdeveloped for EB reactions.     

Formanilide and carbanilide from aniline and carbon dioxide

Earlier syntheses of formamides from the catalytic hydrogenation of CO₂ in the presence of amines were only successful for the preparation of dialkylformamides. After an analysis of the reason for the failure of the reaction using aniline as a starting material, formanilide has been prepared, for the first time, from CO₂, H₂ and aniline with the use of 1,8-diazabicyclo[5.4.0]undec-7-ene. Omission of the H₂ reductant causes the selectivity to switch to the production of carbanilide (1,3-diphenylurea).     

Liquid poly(ethylene glycol) and supercritical carbon dioxide: a benign biphasic solvent system for use and recycling of homogeneous catalysts

Poly(ethylene glycol) (PEG), having a molecular weight of 900 or 1500, is a solid at room temperature but a nonvolatile liquid at 40 degrees C under CO2 pressure. Homogeneously catalyzed hydrogenation can be performed in the molten PEG, followed by extraction of the product by supercritical CO2. The catalyst-containing PEG phase which remains in the vessel can be reused for hydrogenation without addition of further catalyst or PEG.     

Carbon dioxide as a solubility "switch" for the reversible dissolution of highly fluorinated complexes and reagents in organic solvents: application to crystallization

Highly fluorinated organic or organometallic solid compounds can be made to dissolve in liquid hydrocarbons by the application of 20-70 bar of CO(2) gas. Subsequently releasing the gas causes the compounds to precipitate or crystallize, giving quantitative recovery of the solid. The resulting crystals can be of sufficient quality for single-crystal X-ray crystallography; the structures of Rh(2)(O(2)CCF(2)CF(2)CF(3))(4)(DMF)(2), Rh(2)(O(2)C(CF(2))(9)F)(4)(MeOH)(2), Cr(hfacac)(3), and P[C(6)H(3)(3,5-CF(3))(2)](3) have been determined from crystals grown in this manner.     

Determination of antifungal proteins in soil by liquid chromatography

A liquid chromatography method was developed for the determination of antifungal/antimicrobial proteins Rs-AFP1 and Dm-AMP1 in sandy loam soils. The extraction of these highly basic proteins was achieved by mechanical shaking with aqueous Tris buffer pH 9 containing guanidinium thiocyanate salt (4.1 M), EDTA and nonionic polyoxyethylene 20 cetyl ether, Brij-58 detergent. The extracts were cleaned up on Oasis HLB polymer solid-phase extraction cartridges and quantified by liquid chromatography fluorescence detection based on the fluorescence properties of the tryptophan content of these proteins. The detector response was linear for 0.3-10 microg mL(-1). Procedural recoveries were tested in the range 10-100 mg kg(-1). The limit of quantification was 10 mg kg(-1 )protein in the soil sample representing the lowest validated fortification level. The antifungal proteins were found to be stable in soil extract tested up to 9 days when stored at 4 degrees C.     

First observation of the decays B(0) --> D(*-)p_p pi+ and B(0) --> D(*-)p_n

We report the first observation of exclusive decays of the type B-->D(*)N_NX, where N is a nucleon. Using a sample of 9.7x10(6)B_B pairs collected with the CLEO detector operating at the Cornell Electron Storage Ring, we measure the branching fractions B(B0-->D(*-)p_p pi(+)) = (6.5(+1.3)(-1.2)+/-1.0)x10(-4) and B(B0-->D(*-)p_n) = (14.5(+3.4)(-3.0)+/-2.7)x10(-4). Antineutrons are identified by their annihilation in the CsI electromagnetic calorimeter.     

Study of charmless hadronic B meson decays to pseudoscalar-vector final states

We report results of searches for charmless hadronic B meson decays to pseudoscalar( pi(+/-), K+/-, pi(0), or K(0)(S))-vector( rho, K(*), or omega) final states. By using 9.7x10(6) BB pairs collected with the CLEO detector, we report the first observation of B(-)--->pi(-)rho(0), B(0)-->pi(+/-)rho(-/+), and B(-)-->pi(-)omega, which are expected to be dominated by hadronic b-->u transitions. The measured branching fractions are (10.4(+3.3)(-3.4)+/-2.1)x10(-6), (27.6(+8.4)(-7.4)+/-4.2)x10(-6), and (11.3(+3.3)(-2.9)+/-1. 4)x10(-6), respectively. Branching fraction upper limits are set for all of the other decay modes investigated.