生物材料中克伦特罗的气相色谱-质谱法测定

Determination of Clenbuterol in Biological Samples by Gas Chromatography-Mass Spectrometry

建立了生物材料中克伦特罗 (clenbuterol)的气相色谱 -质谱测定方法 ;大白鼠喂食克伦特罗获得阳性生物材料 ,生物材料中克伦特罗经0.01mol/L盐酸溶液提取 ,乙醚脱脂净化 ,乙酸乙酯提取后蒸发至干 ,用乙醇溶解后加样到氧化铝柱上 ,用0.01mol/L盐酸溶液洗脱 ,蒸发至干后 ,用BSTFA(双三甲基硅烷基三氟乙酰胺 ) +1 % (φ)TMCS(三甲基氯硅烷 )衍生 ,采用GC -MS进行测定 ,外标法定量 ;试验表明 ,生物材料中添加0.056×10 -6～0.54×10 -6(w)含量水平的克伦特罗 ,方法回收率在89 %～107 % ,相对标准偏差为7.3 %～16 % ,线性相关系数r为0.998,克伦特罗的检出限为2.0×10-9(w)。

A method for the determination of clenbuterol in biological samples(including liver, lung and muscle) has been developed. Biological samples were obtained by feeding mouses with clenbuterol. The clenbuterol in biological samples was extracted by 0.01 mol/L HCl, defatted by ethyl ether, re _ extracted by ethyl acetate. The extractive was dried out. Dissolved the residual with ethanol, the clenbuterol solution passed through a column of Al2O3, the column then was eluted with 0.01 mol/L HCl. The eluate was evaporated to dryness and derivatized with bis(trimethylsilyl) trifluoroacetamide+1% trimethyl _ chlorosilane. The samples were analyzed by GC-MS with quantitation of external standard method. The recoveries of 89%～107%, RSDs of 7.3%～16%(n=6) and the correlation coefficient of 0.998 were obtained, when clenbuterol was added to the biological samples in 0.056×10-6～0.54×10-6(w) levels. The detection limit of clenbuterol for the method was 2.0×10-9(w).