熟肉制品中4种β-受体激动剂残留量的全自动固相萃取-气相色谱质谱测定法

Determination of fourβ-receptor agonist residues in cooked meat products by automatic-solid phase extraction combined with gas chromatography mass spectrometry

目的利用全自动固相萃取仪对样品进行净化,建立熟肉制品中4种β-受体激动剂气相色谱质谱联用检测方法。方法采用β-葡萄糖苷酸酶/芳基硫酸酯酶37℃酶解样品过夜,全自动固相萃取仪净化,双三甲基硅基三氟乙酰胺+1%三甲基氯硅烷衍生后采用TG-5MS毛细管柱经程序升温分离后进质谱仪检测分析,同位素内标法定量。结果该方法条件下各化合物分离效果良好,曲线相关系数均>0.999,加标回收率为80.12%~90.16%,相对标准偏差为1.98%~6.20%(n=6)。结论本方法前处理快速简便,方法灵敏度高、重现性好,对操作人员及环境相对友好,适用于检测熟肉制品中4种β-受体激动剂残留量。

Objective To purify the samples with automatic-solid phase extraction instrument,and develop a method for determination of fourβ-receptor agonist residues in cooked meat products by gas chromatography mass spectrometry.Methods The samples were firstly digested withβ-glucosidase/arylsulfatase overnight at 37℃,purified with automatic solid phase extraction instrument,derived with Bis(trimethylsilyl)trifluoroacetamide+1%trimethylchlorosilane,separated with TG-5MS capillary gas chromatography column,finally determined by gas chromatography mass spectrometry after separation by temperature programmed,and quantified by internal standard method.Results The method has good separation effect under the conditions,the correlation coefficients of the four target compounds were>0.999,the recoveries were 80.12%-90.16%,and the relative standard deviation(RSD)(n=6)was 1.98%-6.20%.Conclusion The method is fast and simple for pretreatment,with high sensitivity and good reproducibility,and is relatively friendly to operators and the environment,which is suitable for the determination of fourβ-receptor agonist residues in cooked meat products.