固相萃取-高效液相色谱-二极管阵列检测法比较两种不同方法提取牛肝中苯并咪唑类药物及其代谢物。
Comparison of two different isolation methods of benzimidazoles and their metabolites in the bovine liver by solid-phase extraction and liquid chromatography-diode array detection.
机构信息
Dipartimento di Scienze Chimiche, Facoltà di Farmacia, Università di Camerino, via S. Agostino 1, Camerino, Italy.
出版信息
J Chromatogr A. 2010 Mar 12;1217(11):1779-85. doi: 10.1016/j.chroma.2010.01.056. Epub 2010 Jan 25.
A new analytical method that uses high performance liquid chromatography-diode array detector (HPLC-DAD) was developed for the analysis of 14 benzimidazoles residues, including metabolites, in bovine liver. Samples were extracted using two different extraction procedures: with phosphate buffer after enzymatic hydrolysis (method A) or using organic solvent, i.e. acetonitrile (method B). Then, samples were purified on a strong cation exchange (SCX) cartridge and analyzed in HPLC/DAD. The recovery percentages, obtained spiking the matrix (liver) at concentrations of 500 and 100 microg kg(-1) with a standard mixture of benzimidazoles, were in the range 6-101% and 80-102% for methods A and B, respectively. The repeatability of the methods was assessed in all cases by the % of correlation value (CV) that was lower than 19%. The limits of quantification (LOQs) in the matrix for methods A and B were in the range 40-60 and 20-50 microg kg(-1), respectively. The best of the two methods, method B, was used for the analysis of 10 bovine liver samples.
建立了一种采用高效液相色谱-二极管阵列检测法（HPLC-DAD）分析牛肝中 14 种苯并咪唑类药物残留（包括代谢物）的新分析方法。样品采用两种不同的提取方法进行提取：酶解后用磷酸盐缓冲液提取（方法 A）或用有机溶剂（乙腈）提取（方法 B）。然后，样品在强阳离子交换（SCX）柱上进行纯化，并在 HPLC/DAD 中进行分析。用标准混合苯并咪唑类药物在浓度为 500 和 100μg/kg 水平对基质（肝）进行加标，方法 A 和方法 B 的回收率分别在 6-101%和 80-102%范围内。两种方法的重复性均通过相关系数（CV）的%值评估，CV 值均低于 19%。方法 A 和方法 B 在基质中的定量限（LOQs）分别为 40-60 和 20-50μg/kg。对 10 个牛肝样品进行分析，选用了两种方法中最佳的方法 B。
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