College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science of Hebei Province, Baoding, 071002, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jun 15;879(20):1757-63. doi: 10.1016/j.jchromb.2011.04.021. Epub 2011 Apr 22.
A new procedure has been described for the extraction of diclazuril (DIZ), toltrazuril (TOZ) and its two main metabolites toltrazuril sulphoxide (TZSO) and toltrazuril sulphone (TZS) from poultry tissues and eggs, using gel permeation chromatography (GPC). The analytes and the deuterated internal standard were extracted from the samples with ethyl acetate. The analytes were measured by LC coupled to an electrospray ionization tandem mass spectrometer operating in the negative ion mode. Excellent linear dynamic range was observed from 1 to 500 μg/L with the correlation coefficients (R(2)) better than 0.99 for all analytes. The method LOQ of the four analytes in real samples was 1.2 μg/kg for DIZ and TOZ, and 1.8 μg/kg for TZSO and TZS. These values are far lower than the maximum residue limits (MRLs) established by several control authorities. The developed method was accurate with overall recoveries in four matrices.
一种新的程序已经被描述用于从家禽组织和蛋中提取地克珠利（DIZ）、妥曲珠利（TOZ）及其两个主要代谢物妥曲珠利砜（TZSO）和妥曲珠利砜（TZS），使用凝胶渗透色谱（GPC）。分析物和氘代内标物用乙酸乙酯从样品中提取。通过 LC 与电喷雾离子串联质谱仪在负离子模式下进行测量。所有分析物的线性动态范围均为 1 至 500 μg/L，相关系数（R（2））均大于 0.99。在实际样品中，四种分析物的方法 LOQ 为 DIZ 和 TOZ 的 1.2 μg/kg，TZSO 和 TZS 的 1.8 μg/kg。这些值远低于几个控制机构规定的最大残留限量（MRLs）。该方法在四个基质中的总回收率是准确的。
