超高效液相色谱-三重四级杆质谱联用-内标法对豆芽中抗生素的测定  

Determination of antibiotics in bean sprouts by UHPLC-MS/MS-internal standard method

作　　者：张晓艺[1] 郑三燕[1] 张秀尧[1] 李瑞芬[1] 杨舒然 ZHANG Xiaoyi;ZHENG Sanyan;ZHANG Xiuyao;LI Ruifen;YANG Shuran(Wenzhou Center for Disease Control and Prevention,Wenzhou,Zhejiang 325000,China)

机构地区：[1]温州市疾病预防控制中心,浙江温州325000

出　　处：《上海预防医学》2024年第11期1100-1105,共6页Shanghai Journal of Preventive Medicine

基　　金：温州市科技局基础性社会发展科技项目(Y2020545)。

摘　　要：【目的】建立超高效液相色谱-三重四级杆质谱联用(UHPLC-MS/MS)-内标法同时测定豆芽中喹诺酮类、磺胺类、四环素类、大环内酯类和硝基咪唑类抗生素等59种抗生素。【方法】在5.0 g样品中加入内标物、5.0 mL含0.1%甲酸的乙腈,超声提取,提取液过0.22μm滤膜后直接进样1.0μL,以含0.1%甲酸的甲醇溶液和含0.1%甲酸的2.0 mmol·L^(-1)甲酸铵水溶液作为流动相进行梯度洗脱,在ACQUITY PREMIER BEH C18色谱柱上实现分离,采用电喷雾离子源正离子多反应监测模式检测,内标法定量。【结果】豆芽中59种抗生素在10~1000μg·kg^(-1)范围内线性关系良好,黄豆芽的方法检出限为0.1~3.0μg·kg^(-1),定量限为0.4~10.0μg·kg^(-1);绿豆芽的方法检出限为0.1~2.0μg·kg^(-1),定量限为0.4~7.0μg·kg^(-1)。59种抗生素在10、50、200、800μg·kg^(-1)4个添加水平下,黄豆芽的平均回收率为82.1%~122.3%,相对标准偏差为1.2%~15.4%(n=6);绿豆芽的平均回收率为87.3%~119.1%,相对标准偏差为0.9%~15.0%(n=6)。【结论】该方法快速、灵敏和准确,可用于大批量豆芽使用喹诺酮类、磺胺类、四环素类、大环内酯类和硝基咪唑类抗生素的快速筛查。[Objective]To establish an ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)-internal standard method for the simultaneous determination of 59 antibiotics,including quinolones,sulfonamides,tetracyclines,macrolides and nitroimidazole in bean sprouts.[Methods]The internal standard compounds and 5.0 mL of acetonitrile containing 0.1%formic acid were added into 5.0 g of the sample,and then extracted by ultrasonication.The extracted supernatant was filtered by 0.22μm membrane and then injected into 1.0μL of the sample directly.Methanol containing 0.1%formic acid and 2.0 mmol·L^(-1)ammonium formate containing 0.1%formic acid were taken as the mobile phases to conduct gradient elution.The separation was achieved on an ACQUITY PREMIER BEH C18 column.The separated analytes were detected by the electrospray ionization(ESI)in multiple reaction monitoring(MRM)mode,and quantified by internal standard method.[Results]The 59 kinds of antibiotics in bean sprouts had a good linear relationship in the range of 10μg·kg^(-1)to 1000μg·kg^(-1).The limits of detection(LODs)and the limits of quantification(LOQs)of the method for soybean sprouts ranged from 0.1μg·kg^(-1)to 3.0μg·kg^(-1)and 0.4μg·kg^(-1)to 10.0μg·kg^(-1),respectively.While,the LODs and LOQs of the method for mung bean sprouts ranged from 0.1μg·kg^(-1)to 2.0μg·kg^(-1)and 0.4μg·kg^(-1)to 7.0μg·kg^(-1),respectively.The average recoveries of the 59 kinds of antibiotics at four levels(10、50、200、800μg·kg^(-1))in soybean sprouts were 82.1%-122.3%,with the relative standard deviations(RSDs)of 1.2%-15.4%(n=6).However,the average recoveries of the 59 kinds of antibiotics in mung bean sprouts were 87.3%-119.1%,with the RSDs of 0.9%-15.0%(n=6).[Conclusion]The method is rapid,highly sensitive and accurate,which can be used for rapid screening of quinolones,sulfonamides,tetracyclines,macrolides,and nitroimidazole antibiotics in large quantities of bean sprouts.

关 键 词：超高效液相色谱-三重四级杆质谱联用法 磺胺类药 四环素 大环内酯抗生素 喹诺酮类 硝基咪唑 豆芽 

分 类 号：R115[医药卫生—公共卫生与预防医学]