液相色谱-串联质谱法检测食品中残留 - 食品安全质量检测学报.doc

液相色谱-串联质谱法检测中残留 杨翠娜1, 白洪健2, 金 秋2* （1. ××大学食品学院，无锡 2；2. ××××，北京 100083） : 目的 建立一种兽药残留的液相色谱-串联质谱(HPLC-MS/MS)检测方法。方法样品经盐酸甲醇提取液提取, 醋酸铅沉淀蛋白后, 过混合阳离子(MCX)固相萃取柱净化。采用0.1%甲酸(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱, 质谱(ESI+)采用多离子检测模式(MRM)对β2-受体激动剂的定量离子和定性离子进行监测。结果本方法在15 min内完成26种目标化合物的分离分析。26种β2-受体激动剂在、0和0 μg/L添加水平的回收率为72.0%~106.4%, 相对标准偏差小于11.8%(n=6), 方法定量限为10 μg/kg。结论该方法快速、准确、灵敏, 适合测定药物残留。 关键词β2-受体激动剂液相色谱-串联质谱饲料残留 Simultaneous etermination of ……residues in food by liquid chromatography-tandem mass spectrometry YANG Cui-Na1, BAI Hong-Jian2, JIN Qiu2* (1. College of Food Science, ×× University, Wuxi 214122, China; 2. College of Food Science and Nutritional Engineering, ×× University, Beijing 100083, China) ABSTRACT: Objective To determination of in food samples by liquid chromatography -tandem mass spectrometric (LC–MS/MS). Methods Feed samples were extracted with muriatic acid and methanol solution. And then the β2-agonist residues in the extracts were separated on a reversed phase using a gradient elution program of 0.1% formic acid aqueous solution (A) and 0.1% formic acid in acetonitrile solution (B). Using LC–MS/MS (ESI+) with multiple reactions monitoring (MRM), identification of the major components of the 26 kinds of β2-agonist residues was performed based upon the intensities of fragments. Results The recoveries were ranged from 72.0% to 106.4% for the 26 kinds of β2-agonist residues with 3 spiked levels of 20, 50 and 100 μg/kg. The relative standard deviations (RSDs) were less than 11.8% (n=6), and the limits of quantitation (LOQ) for the 26 kinds of β2-agonists were 10 μg/kg. Conclusion The proposed method is fast, accurate and sensitive, which is suitable for detecting β2-agonist residues in feed samples. KEY WORDS: β2-Agonist; high performance liquid chromatography-tandem mass spectrometry; feed; residues 1 引言 β2-兴奋剂临床上主要用于治疗哮喘、支气管痉挛等。此类物质可以增加蛋白质合成、增强体脂分解、显著提高胴体的瘦肉率、增重和饲料转化率, 因此曾被用作牛、羊、禽、猪等畜禽的促生长剂, 俗称“瘦肉精”[1-3]。现代医学实验已证明其残留会严重影响到人类健康, 如果长期食用含有β2-兴奋剂残留的猪肉还会增加致癌、致畸的风