Analysis of suddenly started laminar flow in the entrance region of a circular tube

Suddenly started laminar flow in the entrance region of a circular tube, with constant inlet velocity, is investigated analytically by using integral momentum approach. A closed form solution to the integral momentum equation is obtained by the method of characteristics to determine boundary layer thickness, entrance length, velocity profile, and pressure gradient.Nomenclature M(, , ) a function - N(, , ) a function - p pressure - p* p/1/2U ², dimensionless pressure - Q(, , ) a function - R radius of the tube - r radial distance - Re 2RU/, Reynolds number - t time - U inlet velocity, constant for all time, uniform over the cross section - u velocity in the boundary layer - u* u/U, dimensionless velocity - u ₁ velocity in the inviscid core - x axial distance - y distance perpendicular to the axis of the tube - y* y/R, dimensionless distance perpendicular to the axis - boundary layer thickness - * displacement thickness - /R, dimensionless boundary layer thickness - momentum thickness - absolute viscosity of the fluid - /, kinematic viscosity of the fluid - x/(R Re), dimensionless axial distance - density of the fluid - tU/(R Re), dimensionless time - _w wall shear stress     

Determination of Shikimic Acid in Fruits of Illicium Species and Various Other Plant Samples by LC–UV and LC–ESI–MS

A simple and specific analytical method for the quantitative determination of shikimic acid from the methanol extract of the fruits of Illicium species and from various plant samples was developed. The LC–UV separation was achieved by reversed-phase chromatography on a C18 column with potassium dihydrogen phosphate and methanol as the mobile phase. In the LC–MS method, the separation was achieved by a C12 column using water and acetonitrile, both containing 0.1% acetic acid as the mobile phase. The methods were successfully used to study the percentage compositions of shikimic acid present in nine species of Illicium and various other plant samples. The detector response was linear with concentrations of shikimic acid in the range from 1.0–500.0 μg mL^?1 by LC–UV and 100–1000 ng mL^?1 by LC–MS. Mass spectrometry coupled with electrospray ionization interface is described for the identification of shikimic acid in various plant samples. This method involved the use of the [M-H]^? ions of shikimic acid at m/z 173.0455 (calculated mass) in the negative ion mode with extractive ion monitoring.     

Sulfonic acid functionalized silica as an efficient heterogeneous recyclable catalyst for one‐pot synthesis of 2‐substituted benziimidazoles

An efficient one‐pot synthesis of 2‐substituted benzimidazoles from o‐phenylenediamine and aldehydes in the presence of sulfonic acid functionalized silica at room temperature is reported.     

Rapid analysis of lignans from leaves of Podophyllum peltatum L. samples using UPLC‐UV‐MS

A new rapid UPLC‐UV‐MS method has been developed that permits the analysis of four lignans (4′‐O‐demethylpodophyllotoxin, podophyllotoxin, α‐peltatin and β‐peltatin) in P. peltatum L. Podophyllotoxin is a natural lignan that is being used as a precursor for the semi‐synthetic anti‐cancer drugs etoposide, teniposide and etopophos. The chromatographic separation was achieved using a reversed‐phase C₁₈ column with a mobile phase of water and acetonitrile, both containing 0.05% formic acid. Analyses of P. peltatum leaves collected from different colonies within a single site indicated a significant variation in 4′‐O‐demethylpodophyllotoxin, α‐peltatin, podophyllotoxin and β‐peltatin content. Within 3.0 min four main lignans could be separated with detection limits of 0.1, 0.3, 0.3 and 0.2 μg/mL, respectively. 4′‐O‐demethylpodophyllotoxin and α‐peltatin appeared most prominently among the lignans obtained. The podophyllotoxin content was found in the range of 0.004–0.77% from 16 samples collected from 6 colonies within the same site. The content of podophyllotoxin is directly proportional to the content of 4′‐O‐demethylpodophyllotoxin and inversely proportional to α‐peltatin and β‐peltatin content. LC‐mass spectrometry coupled with electrospray ionization (ESI) interface method is described for the identification of four lignans in various populations of plant samples. By applying principal component analysis and hierarchical cluster analysis, Podophyllum samples collected from various colonies within a location were distinguished. Copyright © 2011 John Wiley & Sons, Ltd.     

Determination of the appetite suppressant P57 in Hoodia gordonii plant extracts and dietary supplements by liquid chromatography/electrospray ionization mass spectrometry (LC-MSD-TOF) and LC-UV methods

Hoodia gordonii is traditionally used in South Africa for its appetite suppressant properties. P57AS3 (P57), an oxypregnane steroidal glycoside, is the only reported active constituent from this plant as an appetite suppressant. Effective quality control of these extracts or products requires rapid methods to determine P57 content. New methods of liquid chromatography/mass spectrometry (LC/MS) and LC-UV for analysis of P57 from H. gordonii have been developed. The quantitative determination of P57 was achieved with a Phenomenex Gemini (Torrance, CA) reversed-phase column using gradient mobile phase of water and acetonitrile, both containing 0.1% acetic acid. The method was validated for linearity, repeatability, and limits of detection and quantification. Good results were obtained in terms of repeatability (relative standard deviation <5.0%) and recovery (98.5-103.5%). The developed methods were applied to the determination of P57 for H. gordonii plant samples, one related genus (Opuntia ficus-indica), and dietary supplements that claim to contain H. gordonii.     

Quantitative determination of seven chemical constituents and chemo‐type differentiation of chamomiles using high‐performance thin‐layer chromatography

A simple and rapid high‐performance thin‐layer chromatographic method was developed for the separation and determination of six flavonoids (rutin, luteolin‐7‐O‐β‐glucoside, chamaemeloside, apigenin‐7‐O‐β‐glucoside, luteolin, apigenin) and one coumarin, umbelliferone from chamomile plant samples and dietary supplements. The separation was achieved on amino silica stationary phase using dichloromethane/acetonitrile/ethyl formate/glacial acetic acid/formic acid (11:2.5:3:1.25:1.25 v/v/v/v/v) as the mobile phase. The quantitation of each compound was carried out using densitometric reflection/absorption mode at their respective absorbance maxima after postchromatographic derivatization using natural products reagent (1% w/v methanolic solution of diphenylboric acid‐β‐ethylamino ester). The method was validated for specificity, limits of detection and quantification, precision (intra‐ and interday) and accuracy. The limits of detection and quantification were found to be in the range from 6–18 and 16–55 ng/band for six flavonoids and one coumarin, respectively. The intra‐ and interday precision was found to be <5% RSD and recovery of all the compounds was >90%. The data acquired from high‐performance thin‐layer chromatography was processed by principal component analysis using XLSTAT statistical software. Application of principal component analysis and agglomerative hierarchial clustering was successfully able to differentiate two chamomiles (German and Roman) and Chrysanthemum.     

Differentiating the gum resins of two closely related Indian Gardenia species, G. gummifera and G. lucida, and establishing the source of dikamali gum resin using high-performance thin-layer chromatography and ultra-performance liquid chromatography-UV/MS

Dikamali is a gum resin obtained from the leaf buds of Gardenia lucida or G. gummifera. There is controversy regarding the botanical source of this gum resin with some stating it to be from G. lucida while others claim it to be from G. gummifera. Analytical methods including UPLC and HPTLC were developed for the qualitative analysis of Gardenia species and various commercial samples. The separation using a UPLC method was achieved within 12.0 min by using C18 column material, a water/acetonitrile mobile phase, both containing formic acid, a gradient system, and a temperature of 40 degrees C. Extensive studies of dikamali collected from various parts of India in comparison with the gum resins collected from G. lucida and G. gummifera clearly indicated that the botanical source of commercially available dikamali is G. lucida, not G. gummifera. The marker compounds isolated from a market sample of dikamali were present only in the gum resin of G. lucida and the compounds isolated from G. gummifera were not present in any of the dikamali samples, confirming the botanical source of dikamali. This work is of utmost importance, given the ambiguity regarding the botanical source of the gum resin dikamali. LC/MS coupled with electrospray ionization is described for the identification and confirmation of nine compounds from various samples of the gum resin. An HPTLC method was also developed for the fast chemical fingerprint analysis of Gardenia samples.     

Quantitative determination of pregnanes from aerial parts of Caralluma species using HPLC-UV and identification by LC-ESI-TOF

An HPLC method was developed for the quantitative determination of five pregnane derivatives from aerial parts of Caralluma species and dietary supplements. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ of five pregnane compounds were found to be in the range of 1-5 and 3-15 microg/mL, respectively, by HPLC using photodiode array detection. This method was applied to the identification of three plant materials of Caralluma species (C. fimbriata, C. umbellate, and C. attentuata) and seven dietary supplements claiming to contain C. fimbriata. An LCIMS coupled with electrospray ionization interface method was used for the identification of compounds and involved the use of [M+Na]+ ions in the positive ion mode with extracted ion chromatogram.     

Design and Synthesis of Some New Benzimidazole Containing Pyrazoles and Pyrazolyl Thiazoles as Potential Antimicrobial Agents

A new class of bis heterocycles‐benzimidazolyl pyrazoles were prepared from the Michael acceptor (E)‐3‐(1H‐benzimidazol‐2‐yl)‐1‐aryl‐prop‐2‐en‐1‐one. The thiamide group was exploited to develop thiazole ring on treatment with p‐fluorophenacyl bromide to get tris heterocycles. All the lead compounds were tested for antimicrobial activity. The compound 7d having nitro substituent on the aromatic ring showed greater antimicrobial activity particularly against Pseudomonas aeruginosa and Penicillium chrysogenum.     

Microwave‐Assisted Synthesis of Novel Spiro Phosphonyl Thiazolo Pyrazole Glycosides as Potential Nematicidal Agents

A series of novel dimethyl 7‐((3aR,5S,6S,6aR)‐6‐((1‐(4‐chlorophenyl)‐1H‐1,2,3‐triazol‐4‐yl)methoxy)‐2,2‐dimethyltetrahydrofuro[2,3‐d][1,3]dioxol‐5‐yl)‐4‐(4‐fluorophenyl)‐9‐oxo‐8‐phenyl‐6‐thia‐1,2,8‐triazaspiro[4.4]non‐2‐en‐3‐ylphosphonate 2a – g were synthesized by the reaction of chalcone derivatives of 2‐((3aR,5S,6S,6aR)‐6‐((1‐(4‐chlorophenyl)‐1H‐1,2,3‐triazol‐4‐yl)methoxy)‐2,2‐dimethyltetrahydrofuro[2,3‐d][1,3]dioxol‐5‐yl)‐3‐phenylthiazolidin‐4‐one 1 with Bestmann–Ohira reagent. The chemical structures of newly synthesized compounds were elucidated by IR, NMR, MS, and elemental analysis. The compounds 2a – g were evaluated for their nematicidal activity against Dietylenchus myceliophagus and Caenorhabditis elegans; compounds 2b , 2c , 2g , and 2f showed appreciable nematicidal activity.