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The method is presented to analyze azaperone and carazolol in pigs kidney. Samples were extracted with acetonitryle. The determination was performed by LC-ESI-MS/MS. The LC was equipped with column Luna C18 Phenomenex. Haloperidol was used as internal standards. The method was validation according to the criteria of Decision Commission No 2002/657/EC. Recoveries for the level 100 microg/kg azaperone and 25 microg/kg carazolol were in the range 91.2-107.0% and 70.8-93.2%. The limit of decision (CCalpha) and detection capability (CCbeta) was respectively 125.9 microg/kg, 160.0 microg/kg for azaperone and 29.3 microg/kg, 33.3 microg/kg. LC-MS/MS technique fulfill the requirements of Decision Commission No 2002/657/EC.

Sedatives and tranquillisers are frequently used to reduce stress during the transportation of food producing animals. The most widely used classes of sedatives include the butyrophenone azaperone, the phenothiazines acepromazine, propionylpromazine, chlorpromazine and the [small beta]-blocker, carazolol. For regulatory control purposes, tolerances for azaperone and carazolol have been set by the European Union as 100 and 25 [micro sign]g kg(-1), respectively. Furthermore, the use of the phenothiazines is prohibited and therefore has a zero tolerance. A method for the detection of residues of five tranquillisers and one [small beta]-blocker using a single ELISA plate has been developed. Kidney samples (2.5 g) were extracted with dichloromethane and applied to a competitive enzyme immunoassay using three polyclonal antibodies raised in rabbits against azaperol, propionylpromazine and carazolol conjugates. In sample matrix, the azaperol antibody cross-reacted 28.0% with azaperone and the propionylpromazine antibody cross-reacted 24.9% with acepromazine and 11.7% with chlorpromazine. In the ELISA, the detection capabilities of the six sedatives, azaperol, azaperone, carazolol, acepromazine, chlorpromazine, and propionylpromazine are 5, 15, 5, 5, 20 and 5 [micro sign]g kg(-1), respectively. The proposed method is a sensitive and rapid multi-residue technique that offers a cost effective alternative to current published procedures, without any concession on the ability to detect sedative misuse.

A fast and simple method for the quantification of a number of tranquilizers and the beta-blocker Carazolol in pork and bovine kidney is described. Extracts are purified/concentrated by a solid phase extraction step and separated on a reversed phase column with an alkaline (ammonia) acetonitrile gradient. The electrospray tandem mass spectrometer is operated in positive ion multireaction monitoring mode. Resulting chromatograms are free of interfering peaks. The recovery is >75% for all analytes and the limit of detection <1 ppb, which is well below the current maximum residue limit for the various compounds., (Copyright 2001 John Wiley & Sons, Ltd.)

A rapid and sensitive multi-residue method was developed to attempt to confirm the presence of the beta-blocker carazolol and the tranquillizers acepromazine, azaperone, chlorpromazine, propionylpromazine and xylazine in pig muscle tissues. The procedure involves determination by liquid chromatography coupled with tandem mass spectrometry. The liquid chromatographic separation was performed on a Symmetry C18 column with gradient elution. A mixture of aqueous buffer, containing 0.01% m/v trifluoroacetic acid (pH 3.5), and acetonitrile at a flow rate of 0.4 ml min-1 was used as the mobile phase. The abundant parent ions [M+ H+] produced by positive electrospray ionisation were selected for collisional dissociation with argon. Fragment ions were recorded with daughter ion scan and multiple reaction monitoring. The analytes were identified unambiguously by assessing retention times and diagnostic ions in meat samples spiked from 50 micrograms kg-1 [maximum residue limit (MRL) for azaperone and azaperol] to 5 micrograms kg-1 (MRL for carazolol).

A multi-residue method for the determination of tranquiliser residues in animal tissue is described. The procedure may be used to determine residues of the tranquilisers acepromazine, azaperone, chlorpromazine, haloperidol, propionylpromazine, xylazine, the metabolite of azaperone, azaperol, and the beta-adrenoreceptor blocking agent carazolol. Existing methods of analysis for tranquilisers are based on ultraviolet and fluorescence detection and have been used for pig kidney analysis. Determination in this method was by high-performance liquid chromatography with electrochemical detection in the screen mode. The enhanced selectivity offered by the electrochemical detector allowed determination in liver extracts, which often give rise to more interferences on chromatographic traces when using conventional methods of detection. The method offers up to a ten-fold improvement in limits of determination over methods using ultraviolet and fluorescence detection. Recoveries and coefficients of variation have been determined in the range 2-25 micrograms/kg in pig kidney and liver. This electrochemical detection method has been used to measure residues in routine surveillance programmes.