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-residue β-agonists in cooked meat by isotope dilution-gas chromatography-tandem mass spectrometry

中文关键词:  β-受体激动剂  熟肉  同位素稀释  气相色谱-串联质谱法

英文关键词:β-agonists  cooked meat  isotope dilution  gas chromatography-tandem mass spectrometry

中文摘要:

      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。

英文摘要:

      Objective To establish a method for determination of residues of β-agonists in cooked meat products by gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The sample was hydrolyzed by β-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.