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目的建立可靠的预处理方法,应用于高效液相色谱-串联质谱(HPLC-MS/MS)法检测猪肉、猪肝中β-受体激动剂。方法动物组织经过β-葡萄糖苷酸酶/芳基硫酸酯酶酶解,酶解液用固相萃取柱净化,采用Waters BEH C_(18)柱(2.1 mm×100 mm,1.7μm),梯度洗脱进行HPLC-MS/MS检测,试验中对固相萃取条件进行优化。结果两种β-受体激动剂在0.5~10.0μg/L范围内响应值与浓度呈良好线性关系,相关系数均大于0.999,采用MCX和SCX两种固相萃取柱净化样品,加标回收率分别为81.4%~121.0%和97.0%~113.4%。沙丁胺醇和莱克多巴胺的检出限分别为0.13、0.14μg/kg,在不同基质浓度下的相对标准偏差(RSD)分别为5.9%~16.2%和6.4%~20.2%。结论采用优化后的固相萃取方法通过HPLC-MS/MS检测,精密度和回收率较为理想,可用于动物源性食品中β-受体激动剂残留的检测。
Objective To establish a reliable pretreatment method for the determination of β-agonists in pork and pork liver by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS). Methods The animal tissues were digested with β-glucuronidase / aryl sulfatase, and the hydrolyzate was purified by solid-phase extraction (SPE) column using a Waters BEH C 18 column (2.1 mm × 100 mm, 1.7 μm) Off-line HPLC-MS / MS detection, the conditions for the optimization of solid-phase extraction. Results There was a good linear relationship between the response and concentration of two β-agonists in the range of 0.5-10.0 μg / L with the correlation coefficients greater than 0.999. The samples were cleaned up by MCX and SCX SPE with spiked recoveries Respectively, from 81.4% to 121.0% and from 97.0% to 113.4%. The detection limits of salbutamol and ractopamine were 0.13 and 0.14 μg / kg, respectively, and the relative standard deviations (RSDs) were 5.9% ~ 16.2% and 6.4% ~ 20.2% at different substrate concentrations. Conclusion The optimized SPE method has better precision and recovery by HPLC-MS / MS. It can be used for the detection of β-agonists in animal-derived foods.