US EPA

7733385 

Journal Article 

Simultaneous determination of residues of diclazuril and toltrazuril in chicken tissues by matrix solid phase dispersion-high performance liquid chromatography/ultraviolet detection 

Qi Ke-Zong; Shi Zu-Hao; Peng Kai-Song; Tu Jian; Zhu Liang-Qiang; Chen Ding-Ding 

2007 

Yes 

Chinese Journal of Analytical Chemistry / Fen Xi Hua Xue
ISSN: 0253-3820 

Chinese Academy of Sciences 

NEW YORK 

35 

11 

1601-1606 

Chinese 

WOS:000252811700012 

An efficient and cost-effective method was developed for the simultaneous determination of the residues of diclazuril and toltrazuril in in chicken tissues matrix solid-phase dispersion ( MSPD) and high-performance liquid chromatography ( HPLC) - ultraviolet detection ( UVD) . The optimal manipulation of MSPD was performed : 0.5 g of homogenate of chicken tissue consisting of the premixed standard solution of diclazuril and toltrazuril was blended with 2 g of C18 bulking agent in a clear-glass mortar. The blended material was transferred to a 10-mL column extractor after standing at ventilated chamber for 2 -5 min. The column extractor was fill with glass cotton, 1.5 g of anhydrous sodium sulfate, the blended material, and 0. 5 g of anhydrous sodium sulfate in sequential order from underlayer to upper layer. And then, the column extractor with previous material was eluted with 8 ml each of three solvents (N-hexane, methanol/water(1 : 4, V/V), and methanol) in sequential order. All fractions were then evaporated to dryness under nitrogen gas at 50. Once dried, samples were dissolved in 0. 5 mL of 0. 05 mol/L phosphate acid/triethylamine buffer-acetonitrile (40 : 60) . After the sample solution was filtrated with filter membrane (0. 22 μm), 20 μL of the sample solution were injected into the HPLC system. Under the optimal chromatographic condition, the diclazuril and toltrazuril were separated on C18 column (250 mm x×4. 6 mm i. d., 5 μm) with 0. 05 mol/L phosphate acid/triethylamine buffer-acetonitrile (40 : 60) as the mobile phase, and flow rate of 1.0 mL/min, then were detected by ultraviolet detector at 240 nm wavelength with 0. 05 of AUFS, the injection volume 20 μL and the column temperature was maintained at 25°C. The linear range for quantitative analysis was between 50 and 1000 ng/g. At the added levels of 50, 500, 1000 ng/g, the recoveries of diclazuril and toltrazuril from chicken tissu ranged from 71. 13% -84. 02% with the relative standard deviations (RSD) in the range of 3. 76% -12. 11%, and the RSDs of intra-and inter-day analyses ranged from 3.70% -6.77% . The detection limits of diclazuril and toltrazuril were 8 and 7 ng/g for muscle respectively, and 10 ng/g for liver and kidney. The quantitation limits of of diclazuril and toltrazuril were 10 and 12 ng/g for muscle respectively, and 15 ng/g for liver and kidney. 

matrix solid phase dispersion; high performance liquid chromatography-ultraviolet detection; diclazuril; toltrazuril; residues; chicken tissue