高效液相色谱-串联质谱法检测鹌鹑蛋及鸽蛋中氯霉素类药物残留

Study on determination of chloramphenicol residues in quail eggs and pigeon eggs by high performance liquid chromatography-tandem mass spectrometry

为建立鹌鹑蛋和鸽蛋中氯霉素(CAP)、甲砜霉素(TAP)、氟苯尼考(FF)及其代谢产物氟苯尼考胺(FFA)多残留同时检测的高效液相色谱-串联质谱法,以乙酸乙酯、乙腈、氨水溶液(体积比为49∶49∶2)提取、净化样品,乙腈饱和的正己烷去脂,用高效液相色谱-串联质谱(HPLC-MS/MS)仪进行分析。以多反应监测模式(MRM)运行,采用正、负离子模式下电喷雾电离,内标法定量,以2 mmol·L^-1乙酸铵-水和2 mmol·L^-1乙酸铵-乙腈溶液为流动相。结果表明:CAP、TAP、FF和FFA分别在0.1~25.0、1.0~150.0、0.3~250.0、1.5~250.0μg·kg^-1浓度范围内,线性关系良好,决定系数均在0.9993以上。4种药物添加水平为定量限、0.5 MRL、1 MRL和2 MRL时,平均回收率为89.30%~105.41%,相对标准偏差均低于3.87%。4种药物的检测限和定量限范围分别为0.04~0.50和0.1~1.5μg·kg^-1。

A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was developed for the simultaneous detection of chloramphenicol(CAP),thiamphenicol(TAP),florfenicol(FF)and its metabolite florfenicol amine(FFA)in quail eggs and pigeon eggs.The sample was extracted with ethyl acetate∶acetonitrile∶aqueous ammonia solution(49∶49∶2,V/V),and degreased with acetonitrile-saturated n-hexane and subjected to HPLC-MS/MS analysis.The system was run in multiple reaction monitoring(MRM)mode,using electrospray ionization in positive and negative ion mode and quantified by internal standard method.The mobile phase was composed of water and acetonitrile,both containing 2 mmol·L^-1 of ammonium acetate.The results showed that CAP,TAP,FF and FFA were in the range of 0.1-25.0,1.0-150.0,0.3-250.0 and 1.5-250.0μg·kg^-1,respectively,the linear relationship was good,and the determination coefficient was above 0.9993.When the added concentration of the four drugs were limits of quantitation(LOQs),0.5 MRL,1 MRL and 2 MRL,the average recovery was 89.30%-105.41%,and the relative standard deviation was lower than 3.87%.The limits of detection(LODs)and LOQs for the four drugs ranged from 0.04 to 0.50 and 0.1 to 1.5μg·kg^-1,respectively.