A new and rapid titration of antimony(III) with potassium dichromate, with iron(II) as inductor

The optimum conditions for the titration of antimony(III) with dichromate, and diphenyl-aminesulphonic acid as indicator, have been established. No iodine catalyst is used; the analytical reaction is based on an induced reaction with iron(II) as inductor. The titration can be done as easily as an iron(II) titration and the end-point is equally sharp. Titrations are possible with 0.01N solutions.     

Development of a liquid chromatography/electrospray tandem mass spectrometry method for confirmation of chloramphenicol residues in milk after alfa-1-acid glycoprotein affinity chromatography

In this work we present a method for confirmatory analysis of chloramphenicol (CAP) in bovine and buffalo raw milk. CAP is extracted in acetonitrile and purified by affinity chromatography on an alpha-1-acid glycoprotein (AAG) column, then is identified and determined by ion-trap liquid chromatography/electrospray ionisation tandem mass spectrometry (LC/ESI-MS/MS) analysis in the negative ion mode. CAP was identified at the minimum required performance limit (MRPL) of 0.30 ppb, by monitoring the [M-H]- ion and at least two product ions, meeting the qualitative and quantitative criteria set by the European Commission in Decision 2002/657/EC for confirmation of prohibited veterinary drugs. The trueness and within-day and between-day repeatability data are also reported. Moreover, the loading capacity of affinity columns towards CAP was tested. This method, based on the molecular recognition between drug and AAG during the purification step to improve sample cleanup, represents a quantitative and repeatable procedure for confirmatory analysis, and fits the requirements for the routine official control of CAP residues in raw milk.     

Reactions of oxiranes with alkali metals: intermediacy of radical-anions

Reaction of oxiranes with alkali metals in aprotic solvents yields a variety of products depending on the nature of the metal and the structure of the oxirane. Deoxygenation to olefins is the major reaction in case of lithium. Rearrangement to carbonyl compounds, reduction to alcohols and formation of dimeric products occur when oxiranes are treated with sodium. All the reactions could be rationalised by a mechanism involving an initial single electron transfer leading to the formation of a radical-anion intermediate.     

Nucleophilic substitution of alkyl halides by zinc salts-32 preparation of tertiary alkyl esters and ethers under non-solvolytic conditions

Zinc salts of carboxylic acids, phenols and alcohols are found to react with tertiary alkyl halides in nonpolar solvents and in presence of a base yielding the corresponding esters and ethers in moderate to good yields.     

Convenient and efficient stereoselective synthesis of (2Z)-2-(chloromethyl)alk-2-enoates using iron(III) or indium(III) chloride

The stereoselective synthesis of (2Z)-2-(chloromethyl)alk-2-enoates has been achieved efficiently and in high yields and in short reaction times from Baylis-Hillman adducts, 3-hydroxy-2-methylene-alkanoates, by treatment with FeCl₃ or InCl₃ at room temperature.     

一种CO2的矿化封存新方法

针对目前CO2矿化封存的研究现状,提出了一种新的CO2矿化封存方法:利用CO2和NH3反应生成三聚氰酸固体,并考察了温度、压力、反应物配比及有无催化剂对三聚氰酸收率的影响。当反应条件为在250℃,22MPa,NH3与CO2反应配比为1∶1.4,反应8h时,最高收率可达到68.3%。此项技术能够与现在工业成熟的富氧燃烧技术联用,实现对CO2的永久性封存,具有经济效益。     

Syntheses of 4-Aryl Chromanes: A Rearrangement Approach

4-Aryl chromanes are synthesized from 4-Aryloxy chromanes via a rearrangement methodology.     

Validation and clinical application of an LC‐ESI‐MS/MS method for simultaneous determination of tolmetin and MED5, the metabolites of amtolmetin guacil in human plasma

A highly sensitive, rapid assay method has been developed and validated for the simultaneous estimation of tolmetin (TMT) and MED5 in human plasma with liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in the positive‐ion mode. A simple solid‐phase extraction process was used to extract TMT and MED5 along with mycophenolic acid (internal standard, IS) from human plasma. Chromatographic separation was achieved with 0.2% formic acid–acetonitrile (25:75, v/v) at a flow rate of 0.50 mL/min on an X‐Terra RP₁₈ column with a total run time of 2.5 min. The MS/MS ion transitions monitored were 258.1 → 119.0 for TMT, 315.1 → 119.0 for MED5 and 321.2 → 207.0 for IS. Method validation and clinical sample analysis were performed as per FDA guidelines and the results met the acceptance criteria. The lower limit of quantitation achieved was 20 ng/mL and the linearity was observed from 20 to 2000 ng/mL, for both the anlaytes. The intra‐day and inter‐day precisions were in the range 3.27–4.50 and 5.32–8.18%, respectively for TMT and 4.27–5.68 and 5.32–8.85%, respectively for MED5. This novel method has been applied to a clinical pharmacokinetic study. Copyright © 2010 John Wiley & Sons, Ltd.     

Simple,efficient, and selective deprotection of phenolic methoxymethyl ethers using silica-supported sodium hydrogen sulfate as a heterogeneous catalyst

A simple and efficient method has been developed for chemoselective deprotection of phenolic methoxymethyl (MOM) ethers using silica-supported sodium hydrogen sulfate as a heterogeneous catalyst. The conversions occur at room temperature, and the yields of the deprotected phenols are excellent. The method is suitable for deprotection of phenolic MOM ethers of multifunctional bioactive natural products.     

Development and validation of a HPLC method for quantification of rivastigmine in rat urine and identification of a novel metabolite in urine by LC‐MS/MS

A sensitive, specific and accurate HPLC method for the quantification of rivastigmine (RSM) in rat urine was developed and validated. The method involves the simple liquid–liquid extraction of RSM and pyridostigmine as an internal standard (IS) from rat urine with tertiary methyl butyl ether. The chromatographic separation of RSM and IS was achieved with 20 mm ammonium acetate buffer (pH 6.5) and acetonitrile (65:35, v/v) delivered at flow‐rate of 1 mL/min on a Kromasil KR‐100. The method was in linear range from 50 to 5000 ng/mL. The validation was done as per FDA guidelines and the results met the acceptance criteria. The method was successfully applied for the quantification of RSM in rat urine. Besides method validation, we have identified two metabolites of RSM in urine. Both the metabolites were characterized by HPLC‐PDA and LC‐MS/MS and it was found that one metabolite is novel. Copyright © 2010 John Wiley & Sons, Ltd.