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

被引:0
|
作者
Qi Ke-Zong [1 ]
Shi Zu-Hao [1 ]
Peng Kai-Song [1 ]
Tu Jian [1 ]
Zhu Liang-Qiang [1 ,2 ]
Chen Ding-Ding [3 ]
机构
[1] Anhui Agr Univ, Sch Anim Sci, Hefei 230036, Peoples R China
[2] Anhui Vet Workstn, Hefei 230022, Peoples R China
[3] Anhui Agr Univ, Ctr Biotechnol, Hefei 230036, Peoples R China
关键词
matrix solid phase dispersion; high performance liquid chromatography-ultraviolet detection; diclazuril; toltrazuril; residues; chicken tissue;
D O I
暂无
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
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 C, 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 degrees C. 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 mu m), 20 mu L of the sample solution were injected into the HPLC system. Under the optimal chromatographic condition, the diclazuril and toltrazuril were separated on C column (250 mm x 4. 6 mm i. d. 5 mu m) 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 mu L and the column temperature was maintained at 25 degrees 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.
引用
收藏
页码:1601 / 1606
页数:6
相关论文
共 11 条
  • [1] Applications of matrix solid-phase dispersion in food analysis
    Barker, Steven A.
    [J]. Journal of Chromatography A, 2000, 880 (01) : 63 - 68
  • [2] Chen Z. L., 2002, VET PHARM, P291
  • [3] *EMEA, 2004, VET MED EV UN TOLT
  • [4] *EMEA, 2004, VET MED EV UN DICL 1
  • [5] *EMEA, 2004, VET MED EV UN DICL 2
  • [6] FONTAINE A, 1994, J AOAC INT, V77, P1359
  • [7] *JECFA, 1998, WHO FOOD ADD SER, V41
  • [8] JOINT FAO/WHO EXPERT COMMITTEE ON FOOD ADDITIVES - JECFA, 1996, WHO FOOD ADD SER, V36
  • [9] Simple determination of residual anticoccidial drugs (diclazuril and nicarbazin) in chicken tissues by HPLC
    Kanda, M
    Ushiyama, K
    Igusa, K
    Murayama, M
    Horie, M
    Hirokado, M
    Miyazaki, T
    [J]. JOURNAL OF THE FOOD HYGIENIC SOCIETY OF JAPAN, 2003, 44 (02): : 110 - 113
  • [10] Qi Y, 2006, CHINESE J ANAL CHEM, V34, P787