【摘要】 建立了一种使用超高效液相色谱-串联质谱联用仪检测罗非鱼血浆和肌肉中丁香酚残留的方法。血浆经甲醇提取,以乙腈和0.1%的氨水为流动相,采用梯度洗脱对待测物进行分离,采用电喷雾离子源(ESI)负离子扫描,多反应监测模式(MRM)测定,外标法定量;肌肉经正己烷提取,HLB固相萃取柱净化,内标法定量。结果表明,在1.0～100.0μg/L线性范围内,丁香酚在罗非鱼血浆中线性良好(r=0.998 5),平均回收率为97.0%～98.9%,相对标准偏差为1.14%～2.21%;在1.0～90.0μg/kg线性范围内,丁香酚在罗非鱼肌肉中线性良好(r=0.999 8),平均回收率为90.2%～95.9%,相对标准偏差为1.91%～5.28%。血浆和肌肉中丁香酚的定量限分别为2.0μg/L和2.0μg/kg。实验结果满足罗非鱼血浆和肌肉中丁香酚残留的检测需求,可为日后丁香酚相关检测研究提供参考。更多还原

【Abstract】 The study aims to establish a method for the determination of eugenol residues in the plasma and muscle of tilapia using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The plasma was directly extracted with methanol. The muscle was extracted with n-hexane and purified by hydrophilic-lipophilic balance(HLB) cartridge. Both of them were separated by a mobile phase of acetonitrile and 0.1% ammonia using gradient elution, and detected by tandem mass spectrometry using multiple reaction monitoring(MRM) in negative ion mode. The plasma sample was determined by an external reference method, and the muscle sample was quantitated with an internal standard method. The results showed that the eugenol from the plasma of tilapia had a good linear relationship(r=0.998 5)in the range of 1.0-100.0 μg/L, the average recovery was 97.0%-98.9%, and the relative standard deviation was 1.14%-2.21%. The eugenol from in the muscle of tilapia had a good linear relationship in the range of 1.0-90.0 μg/kg(r=0.999 8), the average recovery was 90.2%-95.9%, and the relative standard deviation was 1.91%-5.28%. The limits of quantity(LOQs) were 2.0 μg/L in plasma and 2.0 μg/kg in muscle, respectively.It suggested that the established method can meet the requirement for the detection of eugenol residues in the plasma and muscle of tilapia, which could provide reference for relevant studies on the detection of eugenol in future.更多还原