超高效液相色谱-串联质谱法测定水中阿莫西林的残留量
Determination of Amoxicillin Residue in Water by UPLC-MS/MS
摘 要
采用超高效液相色谱-串联质谱法测定水中低含量的阿莫西林残留。将水样用亲水性聚四氟乙烯针式滤器进行过滤,以Kinetex 2.6 μm C18色谱柱为分离柱,以0.01%(体积分数)甲酸溶液-乙腈混合液为流动相进行梯度洗脱,质谱分析中选择电喷雾正离子源和多反应监测模式,用外标法进行定量。阿莫西林的峰面积与其质量浓度在0.020~1.50 μg·L-1范围内呈线性关系,检出限(3S/N)为10 ng·L-1,测定下限(10S/N)为20 ng·L-1。加标回收率在91.3%~105%之间,测定值的相对标准差(n=6)小于6.0%。
阿莫西林
残留
水
UPLC-MS/MS
Amoxicillin
Residue
Water
Abstract
UPLC-MS/MS was applied to the determination of amoxicillin residue in water. After being filtered through PTFE needle type filter, the water sample was separated on a Kinetex 2.6 μm C18 chromatographic column with a mixture of 0.01% (φ) formic acid solution and acetronitrile as mobile phase for gradient elution. ESI+ and MRM were adopted in MS analysis, and external standard method was used for quantification. Linear relationship was found between the peak area and the mass concentration of amoxicillin the range of 0.020-1.50 μg·L-1, with the detection limit (3S/N) of 10 ng·L-1 and the lower limit of determination (10S/N) of 20 ng·L-1. Recovery rates obtained by standard addition method were in the range of 91.3%-105% and RSDs (n=6) were less than 6.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201607009
所属栏目 工作简报
基金项目 南京市卫生局科研项目(YKK15182)
收稿日期 2015/7/8
修改稿日期
网络出版日期
作者单位点击查看
备注林 洁(1984-),女,福建福州人,讲师,博士研究生, 研究方向为天然产物化学。
引用该论文: LIN Jie,LIU Xiang-ping,SUN Wen-fang. Determination of Amoxicillin Residue in Water by UPLC-MS/MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(7): 783～786
林 洁,刘祥萍,孙文芳. 超高效液相色谱-串联质谱法测定水中阿莫西林的残留量[J]. 理化检验－化学分册, 2016, 52(7): 783～786
共有人对该论文发表了看法，其中：
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】LARA F J, OLMO-IRUELA M D, CRUCES-BLANCO C, et al. Advances in the determination of β-lactam antibiotics by liquid chromatography［J］. Trac Trends in Analytical Chemistry, 2012,38:52-66．
【2】陈杖榴.兽医药理学［M］.北京:中国农业出版社, 2001:198-199．
【3】RIEDIKER S, STADLER R H. Simultaneous determination of five β-lactam antibiotics in bovine milk using liquid chromatography coupled with electrospray ionization tandem mass spectrometry［J］. Analytical Chemistry, 2001,73(7):1614-1621．
【4】刘媛,丁岚,谢孟峡,等.动物组织中阿莫西林残留的液相色谱分析方法研究［J］.色谱, 2004,21(6):541-544．
【5】魏东,王存连,梁淑珍,等.牛奶中阿莫西林残留检测方法的研究［J］.江苏农业科学, 2009,37(2):268-269．
【6】肖飞.阿莫西林、硫酸粘杆菌素注射液的制备及其在肉鸡的药动学与残留检测研究［D］.武汉:武汉工业学院, 2009．
【7】黄百芬,任一平,蔡增轩,等.LC-MS/MS测定牛奶中六种青霉素类抗生素残留［J］.中国食品卫生杂志, 2007,19(1):31-35．
【8】KARAGEORGOU E G, SAMANIDOU V F, PAPADOYANNIS I N. Ultrasound-assisted matrix solid phase dispersive extraction for the simultaneous analysis of β-lactams (four penicillins and eight cephalosporins) in milk by high performance liquid chromatography with photodiode array detection［J］. Journal of Separation Science, 2012,35(19):2599-2607．
【9】HUI L, XI X, XUE Y, et al. Simultaneous determination of amoxicillin and prednisolone in bovine milk using ultra-high performance liquid chromatography tandem mass spectrometry［J］. Journal of Chromatography B, 2012,900(900):59-63．
【10】NAGEL O, MOLINA P, ALTHAUS R. Microbial system for identification of antibiotic residues in milk［J］. Journal of Food & Drug Analysis, 2011,19(3):369-375．
【11】罗璇,李宁涛,冯智劼,等.液相色谱-串联质联法测定食品用塑料包装中邻苯二甲酸酯类增塑剂［J］.理化检验-化学分册, 2014,50(12):1544-1546．
【12】HIRSCH R, TERNES T A, HABERER K, et al. Determination of antibiotics in different water compartments via liquid chromatography-electrospray tandem mass spectrometry［J］. Journal of Chromatography A, 1998,815(2):213-223．
【13】GULKOWSKA A, LEUNG H W, SO M K, et al. Removal of antibiotics from wastewater by sewage treatment facilities in Hong Kong and Shenzhen, China［J］. Water Research, 2008,42(1/2):395-403．
【14】杨刚,黄显会,郭春娜,等.高效液相色谱-串联质谱法检测奶中克拉维酸残留［J］.色谱, 2012,30(6):568-571．
【15】李帅鹏,黄显会,许颖,等.高效液相色谱-串联质谱法测定牛(羊)奶中阿莫西林的残留［J］.华南农业大学学报, 2014,35(4):16-21．
【16】王嘉林,邢向伟,赵建颖,等.串联液质法测定牛奶中16种β-内酰胺类抗生素残留的方法开发［J］.中国卫生检验杂志, 2012,22(9):2031-2033．
【2】陈杖榴.兽医药理学［M］.北京:中国农业出版社, 2001:198-199．
【3】RIEDIKER S, STADLER R H. Simultaneous determination of five β-lactam antibiotics in bovine milk using liquid chromatography coupled with electrospray ionization tandem mass spectrometry［J］. Analytical Chemistry, 2001,73(7):1614-1621．
【4】刘媛,丁岚,谢孟峡,等.动物组织中阿莫西林残留的液相色谱分析方法研究［J］.色谱, 2004,21(6):541-544．
【5】魏东,王存连,梁淑珍,等.牛奶中阿莫西林残留检测方法的研究［J］.江苏农业科学, 2009,37(2):268-269．
【6】肖飞.阿莫西林、硫酸粘杆菌素注射液的制备及其在肉鸡的药动学与残留检测研究［D］.武汉:武汉工业学院, 2009．
【7】黄百芬,任一平,蔡增轩,等.LC-MS/MS测定牛奶中六种青霉素类抗生素残留［J］.中国食品卫生杂志, 2007,19(1):31-35．
【8】KARAGEORGOU E G, SAMANIDOU V F, PAPADOYANNIS I N. Ultrasound-assisted matrix solid phase dispersive extraction for the simultaneous analysis of β-lactams (four penicillins and eight cephalosporins) in milk by high performance liquid chromatography with photodiode array detection［J］. Journal of Separation Science, 2012,35(19):2599-2607．
【9】HUI L, XI X, XUE Y, et al. Simultaneous determination of amoxicillin and prednisolone in bovine milk using ultra-high performance liquid chromatography tandem mass spectrometry［J］. Journal of Chromatography B, 2012,900(900):59-63．
【10】NAGEL O, MOLINA P, ALTHAUS R. Microbial system for identification of antibiotic residues in milk［J］. Journal of Food & Drug Analysis, 2011,19(3):369-375．
【11】罗璇,李宁涛,冯智劼,等.液相色谱-串联质联法测定食品用塑料包装中邻苯二甲酸酯类增塑剂［J］.理化检验-化学分册, 2014,50(12):1544-1546．
【12】HIRSCH R, TERNES T A, HABERER K, et al. Determination of antibiotics in different water compartments via liquid chromatography-electrospray tandem mass spectrometry［J］. Journal of Chromatography A, 1998,815(2):213-223．
【13】GULKOWSKA A, LEUNG H W, SO M K, et al. Removal of antibiotics from wastewater by sewage treatment facilities in Hong Kong and Shenzhen, China［J］. Water Research, 2008,42(1/2):395-403．
【14】杨刚,黄显会,郭春娜,等.高效液相色谱-串联质谱法检测奶中克拉维酸残留［J］.色谱, 2012,30(6):568-571．
【15】李帅鹏,黄显会,许颖,等.高效液相色谱-串联质谱法测定牛(羊)奶中阿莫西林的残留［J］.华南农业大学学报, 2014,35(4):16-21．
【16】王嘉林,邢向伟,赵建颖,等.串联液质法测定牛奶中16种β-内酰胺类抗生素残留的方法开发［J］.中国卫生检验杂志, 2012,22(9):2031-2033．
相关信息
