超高效液相色谱-串联质谱法测定鸡蛋中11种喹诺酮类抗生素残留的样品前处理方法优化  

Optimization of sample pretreatment method for determination of 11 quinolone antibiotic residues in eggs by UPLC-MS/MS

作　　者：廖艳华[1] 周劭桓[1] 林文斯[1] 周能志 刘君[1] LIAO Yanhua;ZHOU Shao huan;LIN Wen si;ZHOU Neng zhi;LIU Jun(Guangxi Center for Disease Control and Prevention, Nanning, Guangxi 530028, Chin)

机构地区：[1]广西壮族自治区疾病预防控制中心,广西南宁530028

出　　处：《中国卫生检验杂志》2018年第8期910-914,921,共6页Chinese Journal of Health Laboratory Technology

摘　　要：目的优化并建立UPLC-MS/MS法测定鸡蛋中11种喹诺酮类抗生素残留的样品前处理方法。方法根据文献报道和现行国家标准,对鸡蛋样品喹诺酮类抗生素的提取、沉淀蛋白方式及其在固相萃取柱的净化选择进行比较研究。鸡蛋样品中的喹诺酮药物用Mcllvaine(pH值=4.0)缓冲液提取,高氯酸调解至pH值=2.5沉淀蛋白后离心,上清液经HLB固相小柱净化,最后用C_(18)柱为液相分离色谱柱,以乙腈和0.10%甲酸水为流动相,经电喷雾离子源(ESI^+)电离,多反应监测(MRM)模式的超高效液相色谱-串联质谱检测,定量方法为基质外标法。结果 11种喹诺酮类在2.0 ng/ml^100.0 ng/ml内,线性关系良好,检出限为1.0μg/kg^2.0μg/kg,精密度RSD<10.0%,加标回收率为80.3%~101.6%。结论该方法具有较高的重现性和灵敏度,各项指标均能满足国内外法规的要求,可用于鸡蛋样品中喹诺酮类药物残留的定量和定性检测。Objective To develop a pretreatment method for the simultaneous determination of 11 quinolones residues in egg samples by ultra performance liquid chromatography tandem mass spectrometry （ UHPLC MS/MS）. Methods According to the literature and the current national standard, different methods were compared on the extraction of quinolone, protein precipitation of sample, and the selection of clean up column for egg sample preparation. The target quinolones in eggs were extracted ultrasonically with Mcllvaine solution（ pH 4.0）, and the pH value was adjusted to 2.5 for protein precipitation with perchloric acid. After filtration and eentrifugation, the supernatant was purified with HLB column. Then the sample solution was separated on a Phenomenex Cls column with gradient elution using aeetronitrile -0.10% formic acid as the mobile phase, and detected by UHPLC -MS/MS using positive electrospray ionization（ ESI ~ ） under the multiple reaction monitoring（MRM）. The quantification was carried out by matrix external standard method. Results Eleven kinds of quinolones showed good linearity in the concentration range of 2.0 ng/ml 100.0 ng/ml, the detection limits were within 1.0 Ixg/kg -2.0 Ixg/kg, the RSD values were all 〈 10.0%, and the recoveries ranged from 80.3% to 96.6%. Conclusion This method has good reproducibility and high sensitivity, which can meet the qualitative and quantitative requirements of domestic and foreign legal standards for assaying quinolone residues in egg samples.

关 键 词：鸡蛋 喹诺酮 残留 前处理 超高效液相色谱-串联质谱 

分 类 号：R155.5[医药卫生—营养与食品卫生学]