| Triazine anticoccidial drugs, Diclazuril (DIC) and Tolrtrazuril (TOL), have been widely used in stockbreeding, especially broiler chicken. Consequently, it is necessary to development of adequate analytical procedures to determine triazine anticoccidial drug residues in food of animal origin. Up to now, few investigations have been undertaken, and never a simultaneous determination method of DIC and TOL residues has been developed.The procedures for veterinary residues extraction from animal tissue and those of extract cleanup reported in the literature are widely varied. Being rather time-consuming and complicated, most of them are impractical for testing a large number of samples within a reasonable period of time. In this work, chicken tissue samples were prepared by means of the matrix solid-phase dispersion (MSPD) technique. The technique, which is very simple and fast, permits the simultaneous determination of a number of compounds in a single sample. In the past decade, MSPD has been increasingly applied for the preparation of different biological samples for the determination of residues of veterinary drugs and contaminants. To the best of my knowledge, there also isn't a report on the use of matrix solid phase dispersion to determine triazine anticoccidial drug residues in chicken or other animal tissues. Therefore, the mostly aim of this paper is to develope a method for simultaneous determination of Diclazuril and Tolrtrazuril residues in chicken tissues based on matrix solid-phase dispersion (MSPD) extraction. The results as follow:1. By introduced of orthogonal design, different parameters were optimized, such as component of eluent and washing eluate, the amount of C18 phase or eluent, By evaluate the recoveries of spiked tissues, A residues extraction method based on matrix solid-phase dispersion is developed for the extraction of diclazuril and toltrazuil from chicken tissues: Firstly, tissue sample was minced by means of a mixer, and 0.5 g of the sample was weighed into a glass grinding mortar. A 2g amount of C18 was added to the sample and blended by means of a glass pestle until a homogeneous mixture was obtained. A 2g amount of anhydrous sodium sulfate was inserted at the bottom of the syringe containing a piece of fiberglass, followed by C18/muscle tissue matrix blend, and covered with a filter paper disk. The column content was pushed with a syringe plunger toward the bottom, making sure not to compress it too much. The column was washed with 8 mL of n-hexane and 8 mL of methanol/water (20 + 80). Diclazuril and tolrtrazuril were eluted with 8 mL of methanol into a tube. The eluate was subsequently evaporated on a rotary evaporator to a volume below 0.5 mL and dried up with nitrogen. A 0.5 mL amount of methanol was then added to the dry residues, and the sample was filtered by 0.22μm filtermembrane. And then, 20μL of the filtrate was injected into HPLC/HPCE.2. A simple and rapid method of simultaneous determination of anticoccidial drag residues, Diclazuril (DIC) and Tolrtrazuril (TOL), in chicken tissues has been developed. DIC and TOL were extracted by MSPD technique from chicken liver, muscle, and fat. DIC and TOL were determined by HPLC. Chromatographic condition: C18 column (5μm, 250mm×4.6mm i.d.)with acetonitrile- 0.05 mol/L phosphoric acid/ thriethylamine (60:40) as the mobile phase; column temperature is 20℃; float rate 1.0mL/min; sample size is 20μL; ultraviolet detection at 240nm wavelength. The retention time of DIC and TOL are respectively 8.92 min and 11.04 min. The mean recoveries (n = 5) of DIC and TOL spiked in chicken tissues at the maximum residue levels were 71.41 -84.06% (CV 3.76-11.26%) and71.13 -81.90% (CV 5.22-12.11%), respectively. The detection limits of DCZ and NCZ were 0.008-0.01 and 0.007-0.01 microgram/g, respectively.3. A high performance capillary electrophoresis method for the simultaneous determination of residues of 2 triazine anticoccidial drugs in chicken tissues is described. Optimizations of different parameters were performed. The retention time of DIC and TOL are respectively 7.39min and 7.14mim. The method used 0.5g tissue sample, silica gel as the matrix solid-phase dispersion sorbent, Recoveries at spiked concentrations between 1.0 and 10.0μg·g-1 were between 71.7 and 87.4%. The limits of detection were 0.05-0.1μg·g-1.The methods are simple and rapid and provide simultaneous determination of triazine anticoccidial drags residues in chicken tissues, with acceptable recoveries and repeatability and an adequate limit of determination. |
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