在线富集-超高效液相色谱-线性离子阱串联质谱法测定饮用水中38种抗生素残留  

Determination of 38 antibiotic residues in drinking water by on-line enrichment-ultra high performance liquid chromatography-linear ion trap tandem mass spectrometry

作　　者：赵超群 梁晶晶 李志梅 徐潇颖 刘柱 ZHAO Chaoqun;LIANG Jingjing;LI Zhimei;XU Xiaoying;LIU Zhu(Zhejiang Institute for Food and Drug Control,Key Laboratory of Quality and Safety of Functional Food for State Market Regulation,Zhejiang Provincial Key Laboratory of Quality and Safety of Health Food for Market Supervision,Hangzhou 310052,China;Wenzhou Institute for Food and Drug Inspection,Wenzhou 325000,China)

机构地区：[1]浙江省食品药品检验研究院,国家市场监管重点实验室(功能食品质量与安全),浙江省市场监管保健食品质量安全重点实验室,杭州310052 [2]温州市食品药品检验科学研究院,温州325000

出　　处：《分析试验室》2023年第8期1066-1073,共8页Chinese Journal of Analysis Laboratory

基　　金：浙江省市场监督管理局雏鹰计划核心项目(CY2022227)资助。

摘　　要：建立了在线富集-超高效液相色谱-线性离子阱串联质谱法同时测定饮用水中38种抗生素残留的方法。样品经离心过滤后,先经XBrigde C_(18)Direct Connect HP(30 mm×2.1 mm, 10μm)在线富集,使用Waters sunfire C_(18)(4.6 mm×250 mm, 5μm)色谱柱,以甲醇和0.1%甲酸溶液为流动相进行梯度洗脱。采用电喷雾离子源,以多反应监测触发增强子离子扫描方式进行质谱检测,在线增强子离子扫描(EPI)谱库定性分析,外标法定量。结果表明,饮用水中38种抗生素残留在0.0412~18.5μg/L范围内线性关系良好,线性相关系数均大于0.9898,回收率均在80.6%~123.8%之间,相对标准偏差均大于11%,检出限为0.012~0.14μg/L,定量限为0.041~0.46μg/L。A method for the simultaneous determination of 38 antibiotic residues in drinking water by on-line enrichment-ultra high performance liquid chromatography-linear ion trap tandem mass spectrometry was established.After centrifugation and ultrafiltration,the sample was on-line concentrated by XBrigde C_(18)Direct Connect HP(30 mm×2.1 mm, 10μm).Gradient elution was carried out with methanol and 0.1%formic acid solution as mobile phase,and the target compounds were eluted on Waters sunfire C_(18)(4.6 mm×250 mm, 5μm)chromatographic column for separation.The mass spectrometry detection was carried out by an electrospray ionization source with multiple reaction monitoring triggering enhanced ion scanning mode.Qualitative analysis was conducted by the online EPI library,and the external standard method was used for quantitative analysis.The results showed that the linear ranges of 38 antibiotic residues were 0.0412-18.5μg/L and the correlation coefficients were above 0.9898.The recoveries were between 80.6%and 123.8%and the relative standard deviations were no higher than 11%.The limits of detection were 0.012-0.14μg/L,and the limits of quantification were 0.041-0.46μg/L.

关 键 词：抗生素残留 中心切割 三重四极杆/线性离子阱质谱 饮用水 

分 类 号：TS207.5[轻工技术与工程—食品科学]