固相萃取-气相色谱-串联质谱法测定熟肝制品中7种β-受体激动剂

Determination of sevenβ-agonists in cooked liver products by solid phase extraction with gas chromatography-trandem mass spectrometry

建立了气相色谱-串联质谱(GC-MS/MS)法测定熟肝制品中7种β-受体激动剂的方法。样品经β-葡萄糖醛苷酶/芳基硫酸酯酶酶解,酸除蛋白,正己烷脱脂后,用SLW固相萃取柱净化。洗脱液氮气吹干,甲苯复溶后,用双(三甲基硅基)三氟乙酰胺+1%(φ)三甲基氯硅烷进行衍生,以GC-MS/MS法测定,同位素内标法定量,使用质控样品评价测定结果的准确性。7种β-受体激动剂的标准曲线相关系数均大于0.999 0。方法的检出限为0.03~0.2μg/kg,样品加标平均回收率为80.8%~110.0%,相对标准偏差为1.0%~8.5%(n=6)。该方法高效准确、灵敏度高、重现性好,适用于熟肝制品中7种β-受体激动剂的同时测定。

An analytical method was developed for determination of sevenβ-agonists in cooked liver products by gas chromatography-trandem mass spectrometry(GC-MS/MS).The samples were hydrolyzed byβ-glucuronidase/arylsulfatase,deproteinized by acid,defatted by n-hexane.The solid phase extraction SLW column was used to purify samples.The eluate was dried by nitrogen and reconstituted by toluene.The target compounds were derived by bis(trimethylsilyl)trifluoroacetamide+1%(φ)trimethylchlorosilane,detected by GC-MS/MS,and quantified by isotope internal standard method.Quality control materials were used to appraise the accuracy of determination.The standard curve correlation coefficients of sevenβ-agonists were all more than 0.9990.The detection limits of the method were 0.03-0.2µg/kg,the average recovery rates were 80.8%-110.0%,and the relative standard deviations(RSD)were 1.0%-8.5%(n=6).This method is efficient,accurate,sensitive and repeatable,which is suitable for the simultaneous determination of sevenβ-agonists in cooked liver products.