摘要
检测采用超高效液相色谱-串联质谱法测定牛肉、猪肉中的氨苯砜、N-乙酰氨苯砜。实验试样经80%乙腈水溶液旋涡震荡、超声萃取,用Oasis PRi ME HLB固相萃取小柱通过式净化。采用乙腈—水为流动相,C18反相色谱柱梯度洗脱,电喷雾正离子(ESI+)模式,多反应监测(MRM)进行检测,内标法定量,UPLC-MS检测。实验浓度范围内线性关系良好,相关系数(r2)均大于0.99,回收率范围在80%~113%之间,精密度变异系数RSD<10%,定量下限达1.0μg/kg,可满足牛肉、猪肉中氨苯砜和N-乙酰氨苯砜残留的检测要求,该方法比一般液相质谱法简单、高效。
Utra performance liquid chromatography - tandem mass spectrometry method was adopted to detect dapsone and N - acetyl dapsone residues in beef and pork. The experimental samples were ex- tracted with 80% acetonitrile water solution through vortex shock and ultrasonic extraction, and purified through Oasis PRIME HLB solid phase extraction column. Acetonitrile - water was used as mobile phase, and C18 reversed phase column was used for gradient elution. The positive electrospray ionization （ESI ＋ ） mode and multiple reactions monitoring （MRM） were adopted to detect, internal standard meth- od was used for quantitative determination, and UPLC - MS was adopted to detect. The linear relation- ship was well in experimental concentration range, the correlation coefficient （ r2 ） was higher than 0.99, the recovery rate range was between 80% - 113% , the coefficient of variation of precision RSD was less than 10%, the quantitative lower limit reached to 1.0μg/kg,and it could satisfy with the detecting de- mand of dapsone and N - acetyl dapsone residues in beef and pork. This method was simple and efficient compared to the general liquid mass spectrometry method.
出处
《肉类工业》
2017年第2期30-33,36,共5页
Meat Industry
