瘦肉精检测方法.docVIP

超高压液相色谱-电喷雾串联四极杆质谱法测定猪肉食品中8种β-受体激动剂 孟 娟, 石 莹, 张 晶, 邵 兵* (北京疾病预防控制中心, 食物中毒诊断溯源技术北京市重点实验室, 北京 1000013) 摘 要: 目的 采用超高压液相色谱-电喷雾串连四极杆质谱同时测定猪肉食品中8种β-受体激动剂残留。方法 试样中β-受体激动剂残留经酶解后超声提取, 低温离心后, 上清液用MCX固相萃取柱净化, Waters ACQUITY UPLCTM BEH C18色谱柱分离, 以甲醇(0.1%甲酸水溶液为流动相梯度洗脱, 最后用液相色谱-质谱/质谱进行测定。结果 该方法的平均回收率为75.6~118.7%, 相对标准偏差小于25.0%, 方法的定量限为0.1~0.2 μg/kg。结论 该方法操作简单, 灵敏度高, 重现性良好, 适用于猪肉食品中β-受体激动剂残留的定性与定量检测。 关键词: 超高压液相色谱-串联质谱法; 固相萃取; β-受体激动剂; 食品安全; 兽药残留 Simultaneous determination of eight β-agonists residues in animal food by ultra pressure liquid chromatography-electrospray tandem mass spectrometry MENG Juan, SHI Ying, ZHANG Jing, SHAO Bing (Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Control and Prevention, Beijing 100013, China) ABSTRACT: Objective To develop an analytical method for the determination of eight kinds of β-agonists in animal producing food based on ultra pressure liquid chromatography-electrospray tandem mass spectrometry (UPLC-MS/MS). Methods Samples were enzymatic hydrolysed and extracted by acetic acid buffer (pH 5.2) and then purified and enriched by Oasis MCX solid phase extraction cartridges. The separation was performed on a Waters ACQUITY UPLCTM BEH C18 column (100 mm×2.1 mm i.d., 1.7 μm) with gradient elution using methanol and water containing 0.1% formic acid at a flow rate of 0.3 mL/min. Results Average recoveries of this method for fortified samples ranged from 75.6% to 118.7% with relative standard deviations less than 25.0%. The limits of quantitation (LOQ) for the whole method ranged from 0.1 μg/kg to 0.2 μg/kg. Conclusion Due to its high sensitivity and reproducibility, the method is suitable for the determination of agnoists in animal producing samples. KEY WORDS: Ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS); solid- phase extraction; β-agonists; food safety; veterinary drugs residue 兽药残留问题是影响动物性食品安全的主要因素[1]。在诸多兽药中, β-受体激动剂因较强的毒性及易被滥用等特点一直受