同位素稀释-气相色谱-串联质谱法测定熟肉中多组分β-受体激动剂

Determination of multi-residueβ-agonists in cooked meat by isotope dilution-gas chromatography-tandem mass spectrometry

目的建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)检测熟肉制品中多种β-受体激动剂残留量的方法。方法样品经β-葡萄糖醛苷酶/芳基硫酸酯酶酶解,酶解液通过MCX固相萃取柱浓缩净化,后用5%氨化乙酸乙酯洗脱,经过双三甲基硅基三氟乙酰胺+1%(φ)三甲基氯硅烷衍生,用GC-MS/MS测定,同位素内标法定量。结果β-受体激动剂在0.05~1 mg/L浓度范围内,线性关系良好,相关系数r>0.9994,回收率为80.3%~109.5%,精密度(RSD)在10%以内。结论该方法精密度好、灵敏度高,可简便、准确地测定熟肉中多种β-受体激动剂的残留量。

Objective To establish a method for determination of residues ofβ-agonists in cooked meat products by gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods The sample was hydrolyzed byβ-glucuronidase/arylsulfatase,concentrated and purified by MCX solid phase extraction column,eluted with 5%ammoniated ethyl acetate,and derivatized with bis(trimethylsilyl)-trifluoroacetamide+1%(φ)trimethylchlorosilane,and then determined by GC-MS/MS,and quantified by isotope internal standard method.Results The linear relationship ofβ-agonist was good in the range of 0.05-1 mg/L,the correlation coefficient r>0.9994,the recoveries were 80.3%-109.5%,and the relative standard deviations(RSDs)were 2.1%-7.6%.Conclusions The method is accurate and sensitive,and can be used for the determination of residualβ-agonists in cooked meat.