Aldehyde determination

By : razan almaaz

Glutaraldehyde
In spite of the inherent limitations of chemical fixation, glutaraldehyde is unsurpassed in its ability to preserve cell ultrastructure. This achievement is due to the introduction of irreversible intra-and intermolecular cross-links into cellular proteins by the dialdehyde. Glutaraldehyde is very effective in stabilizing surface as well as intracellular structures for conventional scanning and transmission electron microscopy and high voltage electron microscopy. Even in immunocytochemical and autoradiographical studies, glutaradehyde plays a dominant role. Furthermore, prior to freeze-substitution, freeze-drying and freeze-fracturing, specimens often are stabilized with this dialdehyde Aqueous solutions of glutaraldehyde used for the chemical modification and stabilization of proteins have been found to consist of free glutaraldehyde (I), the cyclic hemiacetal of its hydrate (II) and oligomers of this (III) in equilibrium with each other. Ultraviolet absorption spectra of these solutions at wavelengths greater than 200 nm should have only a single maximum at 280 nm. Absorption at 235 nm is due to an impurity which can be removed by various means. Reactions of the reagent with proteins involve principally the lysinyl (and hydroxylysinyl) residues in the relative amounts of four moles of glutaraldehyde to one of lysine. Three unstable products can be partially isolated from acid hydrolyzates of glutaraldehydetreated proteins or from the reaction mixtures of glutaraldehyde and model compounds; two of these products have strong ultraviolet absorption near 265 nm

Studies of aqueous solution of glutaraldehyde by capillary gas chromatography-mass : spectrometry

Commercial aqueous solution of glutaraldehyde which consists of products arose from glutaraldehyde have been analysed by capillary gas chromatography (GC) and capillary gas

chromatography-mass spectrometry (GC-MS). The gas chromatographic seperations of aqueous solutions were carried out well on SE-54 coated fused silica capillary column. The capillary GC-MS analyses were performed by electron impact (EI) , field ionization (FI) and chemical ionization (CI) mode using ammonia, isobutane, ammonia-pyridine and isobutanepyridine as the reactant gases. The ammonia CI mass spectra provided the best information for the identification of products in the aqueous solution. The several products formed by aldol .condensation and hydration-polymerization were identified

Benzaldehyde
Abstract :
A simple, precise and accurate capillary gas_/liquid chromatographic procedure has been developed to determine benzaldehyde, the toxic oxidation product of the widely used preservative and co-solvent benzyl alcohol, in injectable formulations of the non-steroidal anti-inflammatory drugs, diclofenac and piroxicam, as well as in Vitamin B-complex injection solutions. Following liquid_/liquid extraction with chloroform, separation and quantification are achieved on a fused silica capillary column (25 m_/0.53 mm i.d.) coated with 0.5 mm film of OV-101. 3-Chlorobenzaldehyde was used as internal standard with flame-ionization as the detection mode. The ability of the system to resolve benzaldehyde peak from interfering components is good. The method displays excellent linearity over the concentration range 0.5_/ 100 mg/ml of benzaldehyde. The quantification limit for benzaldehyde is 0.4 mg/ml.

Instrumentation :
The method was developed on a Shimadzu gas chromatograph Model GC-15A (Shimadzu, Kyoto, Japan) equipped with a flame-ionization detector and a model GC-R4A Chromatopac integrating recorder. The column used was a 25 m_/0.53 mm i.d. fused silica capillary column coated with 0.5 mm film of OV-101. The column, injector and detector temperatures were 160, 270 and 270 8C, respectively. The carrier gas was extra pure helium at a flow rate of 4.5 ml/min. The injection volume was 1 ml and the samples were injected in the split-less mode with a Hamilton syringe

Conclusion :
The GLC method proposed for selective quantitation of neurotoxic benzaldehyde is suitable for application to the quality control analysis of benzyl alcohol containing injection formulations such as Na-diclofenac, Piroxicam and Vitamin Bcomplex. The extraction procedure is straightforward and a moderate analysis time is achieved at the concentration levels involved (1.0_/100 mg/ml) without the need for solvent evaporation. The method validation demonstrated good precision, specificity and accuracy with acceptable recovery and chromatographic resolution.

formaldehyde
: Introduction
Formaldehyde is used in the cosmetic industry as a preservative. Its use is regulated by the European Community, the maximum allowed concentration expressed as free formaldehyde being 0.1% for cosmetics used for oral care, and 0.2% for all the rest .It is also used in the pharmaceutical industry due to its properties as an antiseptic and antimycotic agent. Various methods have been reported in the literature dealing with the determination of formaldehyde in those kinds of samples,mainly based on liquid chromatography, but also gas chromatography spectrophotometry, and capillary electrophoresis .All of them require a more or less complex treatment of the sample, as homogenisation, a derivatisation .reaction, extraction step, etc In the present work, formaldehyde, removed by pervaporation, The stream leaving the unit was mixed with a sulfite solution to yield the coloured product, which was spectrophotometrically monitored at 578 nm. The method was applied to the determination of the analyte in liquid, solid and semisolid samples such as cosmetics and pharmaceutical products, . without any previous treatment

Determination of formaldehyde in liquid, solid and semisolid pharmaceuticals and cosmetics by flow injection-pervaporation:

A spectrophotometric method is proposed for the determination of formaldehyde in liquid, solid and semisolid cosmetic and pharmaceutical samples, employing, for the first time in this field, the coupling of a continuous flow configuration to a pervaporation unit. The method is based on the reaction of the analyte with pararosaniline in acidic medium and subsequent formation of a coloured product (alkylsulfonic acid chromophore) with sodium sulfite, which was monitored spectrophotometrically. The method was applied to samples in which the formaldehyde content is regulated by law.

Reagents :
Ultrapure water obtained from a Milli-Q system (Millipore, Bedford, MA, USA) was used throughout. Aqueous standard solutions both for optimisation and calibration were prepared from formaldehyde (Merck, Darmstadt, Germany), which was standardised iodometrically.23 A 0.05 mol l21 Na2SO3 solution was prepared daily by dissolving the necessary amount of the anhydrous product (Merck) in water. A 2 g l21 pararosaniline (Fluka, Buchs, Switzerland) in 2% (v/v) ethanol (Normasolv, Scharlau, Barcelona, Spain) and 0.5 mol l21 H2SO4 (Merck) was also prepared.

Manifold and procedure for liquid samples :

2 ml of either the standard solution or the diluted sample, was injected (valve IV1) into the water stream and was chanelled to the lower part of the pervaporation unit, which was thermostated at the required temperature . Simultaneously, valve IV2 was switched to the filling position. The volatile analyte evaporated and diffused through the hydrophobic membrane and was accepted by the static acceptor pararosaniline solution. After a 5 min interval for collection of

Manifold and procedure for semisolid and solid samples :

An appropriate amount of the sample was accurately weighed in the lower chamber of the pervaporation module. 0.5 ml of water and 1 ml of formaldehyde standard solution were added. The cell was closed, after fixing in place a 5 mm thickness spacer, between the membrane support and the upper chamber. The acceptor stream was then introduced into the upper chamber and

the baseline was established. The injection valve IV2 was then switched to the filling position. The whole module was placed in a thermostated magnetic stirrer. After 10 min, the valve was switched to the injection position and the signal was finally recorded. This process can not be classified as continuous but as a hybrid between a continuous procedure (collection of the analyte in the acceptor chamber, performance of the chemical reaction and transportation of the product to the detector), and a batch one (preparation of the cell, weighing of the sample and addition of the water and standard solution).
References
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