9-Bromomethylacridine a Novel Fluorescent Labeling Reagent of Carboxylic Group for HPLC

Abstract

9-Bromomethylacridine (9-Br · Ma) gave blue fluorescent 9-acridinylmethyl (9-AM) esters by the reaction with carboxylic acids. The reactions were performed simply by mixing the 9-Br · Ma, tetraethylammonium carbonate (TEA C) and carboxylic acids in N,N-dimethylformamide at room temperature. The 9-AM derivatives of fifteen kinds of fatty acids were separated and detected with high performance liquid chromatography. By this method, fatty acids could be determined at levels down to either pmol order by fluorometry or 10 pmol order by UV method. After saponification, those in triacylglycerols were also determined. When four kinds of fatty acids were added to a butter, their recoveries were 92–101%. The coefficient of variation of myristate as a representative was 2.5% (42.8 pmol, n=6).     

Two new guaianolide-type sesquiterpenoids from Kadsura interior

Two new guaianolide-type sesquiterpenoids,4β,9β-dihydroxy-1α,5α-H-guaia-6,10(14)-dien(1) and 4β,9β,10α-trihydroxy-1α,5α-H-guaia-6-en(2),along with four known sesquiterpenoids(3a,3b,4 and 5),were isolated from Kadsura interior.Their structures and configurations were elucidated by spectroscopic methods including 2D-NMR and HR-MS techniques.Compounds 3a and 3b were obtained as a pair of enantiomers,and their structure and absolute configuration were established from their extensive NMR spectra and by single-crystal X-ray analysis.     

1,3‐Dichloro‐tetra‐n‐butyl‐distannoxane: a new application for catalyzing the direct substitution of 9H‐xanthen‐9‐ol at room temperature

1,3‐Dichloro‐tetra‐n‐butyl‐distannoxane was firstly used to catalyze the direct substitution of 9H‐xanthen‐9‐ol with indoles at room temperature to afford a class of 3‐(9H‐xanthen‐9‐yl)‐1H‐indole derivatives in good to excellent isolating yield. Moreover, other nucleophiles (such as diketone and pyrrole) could also proceed smoothly in this methodology. Copyright © 2012 John Wiley & Sons, Ltd.     

A novel fast method for aqueous derivatization of THC,OH‐THC and THC‐COOH in human whole blood and urine samples for routine forensic analyses

A novel aqueous in situ derivatization procedure with propyl chloroformate (PCF) for the simultaneous, quantitative analysis of Δ⁹‐tetrahydrocannabinol (THC), 11‐hydroxy‐Δ⁹‐tetrahydrocannabinol (OH‐THC) and 11‐nor‐Δ⁹‐tetrahydrocannabinol‐carboxylic acid (THC‐COOH) in human blood and urine is proposed. Unlike current methods based on the silylating agent [N,O‐bis(trimethylsilyl)trifluoroacetamide] added in an anhydrous environment, this new proposed method allows the addition of the derivatizing agent (propyl chloroformate, PCF) directly to the deproteinized blood and recovery of the derivatives by liquid–liquid extraction. This novel method can be also used for hydrolyzed urine samples. It is faster than the traditional method involving a derivatization with trimethyloxonium tetrafluoroborate. The analytes are separated, detected and quantified by gas chromatography–mass spectrometry in selected ion monitoring mode (SIM). The method was validated in terms of selectivity, capacity of identification, limits of detection (LOD) and quantification (LOQ), carryover, linearity, intra‐assay precision, inter‐assay precision and accuracy. The LOD and LOQ in hydrolyzed urine were 0.5 and 1.3 ng/mL for THC and 1.2 and 2.6 ng/mL for THC‐COOH, respectively. In blood, the LOD and LOQ were 0.2 and 0.5 ng/mL for THC, 0.2 and 0.6 ng/mL for OH‐THC, and 0.9 and 2.4 ng/mL for THC‐COOH, respectively. This method was applied to 35 urine samples and 50 blood samples resulting to be equivalent to the previously used ones with the advantage of a simpler method and faster sample processing time. We believe that this method will be a more convenient option for the routine analysis of cannabinoids in toxicological and forensic laboratories.     

DanHong Injection inhibits the development of primary abdominal aortic aneurysms in apoE knockout mice

Clinical observations indicate that DanHong Injection （DHI） can increase blood flow and reduce various syndromes in patients with cardiovascular disease. How- ever, it still needs to define the function of DHI and the involved mechanisms in details, such as the protective effect on the development of primary abdominal aortic aneurysms （AAAs）. In this study, we determined whether DHI is able to inhibit AAA in apoE knockout （apoE-/-） mice. Thirty apoE-/- male mice on high-fat diet （0.5 % cholesterol, 21% fat） were randomly divided into two groups and received i.p. injection of saline （100 μL/day） and DHI （100 μL/day）, respectively, for 16 weeks. At the end of experiment, we determined the development of atherosclerosis in en face aorta and aneurysms,pathological morphology of arterial wall, and serum lipid levels. We also determined the expression of monocyte chemoattractant protein-1 （MCP-1）, MMP-2, and MMP-9 mRNA in aortic wall using real-time RT-PCR. Our results indicated that high-fat diet induced the development of AAAs in apoE-/- mice, but the induction was totally blocked by DHI （P 〈 0.01）. The result of staining of abdominal aortic cross sections showed that DHI main- tained the collagen content in arterial wall, thereby pre- venting the animals from the development of AAA. Although DHI had little effect on serum total- and LDL- cholesterol levels, it reduced the expression of MCP-1, MMP-2, and MMP-9 mRNA in aortic wall （P 〈 0.01）. Taken together, our study suggests that DHI can inhibit the high-fat diet-induced AAA formation. The inhibitory effects may be related to the maintenance of the collagen content and inhibition of expression of AAA-related genes. Our study may suggest a new application of DHI in clinics.     

A comparative study on low‐order,amplitude‐equation and perturbation approaches in thermal convection

A comparison among three weakly nonlinear approaches for thermo‐gravitational instability in a Newtonian fluid layer heated from below is presented. First, the dynamical systems describing the time evolution of the problem from different weakly nonlinear approaches, namely, the Lorenz model, the amplitude equations and the perturbation expansion approaches are obtained. Next, the steady states and their stability, as well as the transient behaviour are obtained from each dynamical system. The similarity and difference among the three models are emphasized. The role of each of the nondimensional groups, the Rayleigh number and the Prandtl number is compared for the three models. The different approaches lead to similar behaviours when the Rayleigh number is just above its critical value and Prandtl number is high. However, only the dynamical system obtained from the amplitude equations is able to reflect the role of the Prandtl number. On the other hand, the amplitude equations and perturbation expansion techniques are not suitable for predicting the uniform oscillatory behaviour observed frequently in Rayleigh–Bénard convection. The novelty of the current work lies in studying the critical differences in the findings of the three popular approaches to investigate weakly nonlinear thermal convection for the first time. Copyright © 2011 John Wiley & Sons, Ltd.     

On the rate of change of the sharp constant in the Sobolev–Poincaré inequality

The rate of change of the sharp constant in the Sobolev–Poincaré or Friedrichs inequality is estimated for a Euclidean domain that moves outward. The key ingredients are a Hadamard variation formula and an inequality that reverses the usual Hölder inequality.