摘要
采用同位素内标-超高效液相色谱串联三重四极杆质谱法测定野拔子蜂蜜中林可霉素残留量。样品经Tris缓冲液(pH 9)提取,Oasis HLB固相萃取柱净化,采用ZORBAX SB-C18色谱柱分离,以0.1%的甲酸水溶液和乙腈为流动相进行梯度洗脱;采用电喷雾-正离子多反应监测模式检测,同位素内标法定量。当林可霉素的浓度为1.0~100.0 ng/mL时,线性关系良好,相关系数(r)>0.999,空白样品的3个添加水平(0.5,2.0和5.0μg/kg)的回收率为91.2%~96.7%,RSD为8.6%~11.8%(n=6),定量限为0.6μg/kg,检出限为0.2μg/kg。说明该方法灵敏度及准确度良好,能满足野拔子蜂蜜中林可霉素残留分析的要求。
To determine lincomycin residues in honey of Elsholtzia rugulosa by ultra-performance liquid chromatographytriple quadrupole mass spectrometry(UPLC-MS/MS)with isotope-labelled internal standards,samples were extracted with tris buffer(pH 9),and cleaned up on a Oasis HLB cartridge.The target analytes were separated on a ZORBAX SB-C18 column with gradient elution using a mobile phase made up of 0.1%formic acid solution and acetonitrile.Detection was carried out using positive electrospray ionization and multiplereaction monitoring(MRM),and quantified with isotope internal standard method.The lincomycin showed a good linearity in the range of 1.0-100.0 ng/mL(r>0.999).The spiked recovery rate was in the range of 91.2%-96.7%at 3 spiked levels(0.5,2.0 and 5.0μg/kg)for blank sample,and the relative standard deviation(RSD)was 8.6%-11.8%(n=6).The limits of detection and limit of quantitation were 0.2μg/kg and 0.6μg/kg,respectively.The method was sensitive and accurate.It could meet the requirements for the determination of lincomycin residues in honey of Elsholtzia rugulosa.
作者
田金凤
尚远宏
郑毅
TIAN Jinfeng;SHANG Yuanhong;ZHENG Yi(Panzhihua University,Panzhihua 617000)
出处
《食品工业》
CAS
北大核心
2019年第10期293-295,共3页
The Food Industry
基金
国家青年科学基金项目（31402237）
西华大学食品生物技术省高校重点实验室开放课题（szjj2017-110）
攀枝花市社会发展科技计划项目（2016 CY-S-10,2018CY-S-28）
