Determination of urea in pet feed: assessing the suitability of different analytical techniques using proficiency test data.

The determination of urea in pet feed at contaminant levels using the spectrophotometric method described in Commission Regulation (EC) No 152/2009 has been reported by several EU laboratories to lack the required selectivity. Whilst urea is not authorised as an additive in pet feed, the control of urea in pet feed is of economic importance, because the addition of urea may unlawfully increase the apparent protein content. To investigate the capabilities of different analytical techniques, a proficiency test was organised where the participants (EU official control laboratories, laboratories from the academia and private laboratories) were free to use their method of choice for analysing three dog feed test materials, two samples of which were spiked with urea.

Proficiency test on the determination of polyethylene and polybutylene terephthalate cyclic oligomers in a food simulant.

The outcome of a proficiency test (PT) organised by the European Union Reference Laboratory for Food Contact Materials (EURL-FCM) is presented. The PT was set up to assess the analytical performance of National Reference Laboratories (NRLs) and Official Control Laboratories (OCLs) in the determination of mass fractions of polyethylene terephthalate (PET) and polybutylene terephthalate (PBT) cyclic dimers and trimers in the official food simulant D1 containing ethanol and water (50:50 v/v). The EURL-FCM had developed and validated an analytical method based on HPLC-UV to monitor the homogeneity and stability of the target oligomers in the PT test items and to determine the respective assigned values, as prescribed in ISO 17043, 2010ISO 17043, 2010.

State of the art in the determination of trace elements in seawater: a worldwide proficiency test.

This manuscript presents the results of the International Measurement Evaluation Programme 40 (IMEP-40) study, a proficiency test (PT) which was organised to assess the worldwide performance of laboratories for the determination of trace elements in seawater. This PT supports the implementation of the European Union Water Framework Directive 2000/60/EC, which aims at achieving a long-term high level protection of the aquatic environment, covering lakes, ground water and coastal waters. Forty-six participants reported results.

Review of analytical methods for the determination of pesticide residues in grapes.

This review presents an overview of analytical methods for the analysis of pesticide residues in grapes and by-products in the last decade. The most widely used detection technique for the determination of pesticides in grapes is mass spectrometry combined with gas and/or liquid chromatography. In general, multi-residue methods with selective sample treatment methodologies have been developed for this purpose.

Proficiency test on the determination of pesticide residues in grapes with multi-residue methods.

This manuscript presents the results of the International Measurement Evaluation Programme 37 (IMEP-37) study, a proficiency test (PT) which was organised to assess the world-wide performance of food control laboratories on the determination of pesticide residues in grapes. This PT supports the implementation of Regulation (EC) No 396/2005 on maximum residue levels of pesticides in or on food and feed of plant and animal origin. Eighty-one participants reported results, forty from EU Member States and forty-one from outside the EU.

Precision study on capillary electrophoresis methods for metacycline.

A CE method for metacycline (MTC) determination was investigated in an inter-laboratory experiment. Many problems were encountered in this study, most of which were related to the transfer of the method to different CE equipment. The reported problems could be classified into different categories: problems related to the precision, to the parameters in the protocol, and to the MTC peak shape.

Investigation of degradation products in a topical gel containing erythromycin and benzoyl peroxide by liquid chromatography-mass spectrometry.

Benzamycin, combining benzoyl peroxide and erythromycin, is a topical gel used in the treatment of acne vulgaris. Because of the reactivity of benzoyl peroxide, preparations containing both erythromycin and benzoyl peroxide might be unstable and degradation products could be formed. To investigate and identify these latter products, a gradient-based liquid chromatographic method using volatile mobile phase constituents was developed.

Facilitated column selection in pharmaceutical analyses using a simple column classification system.

In this paper, the performance of a previously developed classification system applied to pharmaceutical chromatographic analyses, is investigated. The separation of seven different drug substances from their respective impurities was studied. The chromatographic procedure for acetylsalicylic acid, clindamycin hydrochloride, buflomedil hydrochloride, chloramphenicol sodium succinate, nimesulide and phenoxymethylpenicillin was performed according to the corresponding European Pharmacopoeia (Ph.

Intermediate precision study on a capillary electrophoretic method for chlortetracycline.

We describe an intermediate precision study on a capillary electrophoretic (CE) method for chlortetracycline. It is shown how in one setup the influence of the factors time, analyst, and equipment on the precision can be investigated. As different types of CE equipments were included, the transferability of the method could be examined.

Characterisation of reversed-phase liquid-chromatographic columns by chromatographic tests comparing column classification based on chromatographic parameters and column performance for the separation of acetylsalicylic acid and related compounds.

Selection of RP-LC columns with suitable selectivity for a given analysis is difficult. For example, the European Pharmacopoeia (Ph. Eur.

Characterisation of reversed-phase liquid chromatographic columns by chromatographic tests. Rational column classification by a minimal number of column test parameters.

The European Pharmacopoeia (Ph. Eur.) and other official compendia give only a general description of the stationary phase in the description of a liquid chromatographic method.