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目的:建立牛肉中9种β-受体激动剂的UPLC-MS/MS分析方法,为食品安全监测提供数据支撑。方法:样品用β-葡萄糖醛苷酶酶解4 h,高氯酸沉淀除杂,调节pH后,过MCX固相萃取小柱净化,氮气吹干后甲酸溶液复溶,进行UPLC-MS/MS分析。色谱柱:BEH C18(50 mm×2.1 mm,1.7μm);流动相:0.1%甲酸乙腈溶液(A)-0.1%甲酸水溶液(B),梯度洗脱(0~1 min,维持5%A;1~3 min,5%A线性变化至50%A;3~4 min,50%A线性变化至60%A;4~5 min,60%A线性变化至99%A;5~5.5 min,99%A线性变化至5%A;5.5~7.5 min,维持5%A);流速:0.4 mL·min-1;柱温:30℃;进样量:10μL。结果:9种β-受体激动剂在0.5~10.0μg·kg-1添加浓度范围内线性关系良好,相关系数r≥0.9990,较高浓度时回收率范围为62.7%~107.9%,定量下限(LLOQ)规定为添加回收试验中S/N≥10时的最低添加浓度,结果均小于0.5μg·kg-1。结论:经方法学验证,本方法专属性好,简便、准确、快速,适用于牛肉中β-受体激动剂的检测。
OBJECTIVE: To establish a UPLC-MS / MS method for the determination of nine β-agonists in beef, providing data support for food safety monitoring. Methods: The samples were digested with β-glucuronidase for 4 h, perchloric acid precipitates were removed and the pH was adjusted. After purification by MCX solid phase extraction cartridge and formic acid solution by nitrogen gas drying, UPLC-MS / MS analysis. The mobile phase consisted of 0.1% formic acid in acetonitrile (A) and 0.1% formic acid in water (B), gradient elution (0 ~ 1 min, maintaining 5% A; 1 to 3 min, 5% A to 50% A linearly; 3 to 4 min, 50% A linear to 60% A; 4 to 5 min, 60% A linear to 99% 99% A linear change to 5% A; 5.5 ~ 7.5 min, maintaining 5% A); flow rate: 0.4 mL · min-1; column temperature: 30 ℃; injection volume: 10μL. Results: Nine kinds of β-agonists had a good linearity in the concentration range of 0.5 ~ 10.0μg · kg-1 with a correlation coefficient of r ≥ 0.9990. The recoveries ranged from 62.7% to 107.9% at higher concentrations. The lower limit of quantitation LLOQ) is defined as adding the recovery test S / N ≥ 10 minimum concentration, the results were less than 0.5μg · kg-1. Conclusion: The method is validated by the method, the method is specific, simple, accurate and rapid, suitable for the detection of beta-agonists in beef.