色谱

色谱 ›› 2012, Vol. 30 ›› Issue (10): 1089-1092.DOI: 10.3724/SP.J.1123.2012.06030

• 技术与应用 • 上一篇    

高效液相色谱-串联质谱法测定蜂蜜中的阿莫西林残留量

许蔚*, 张晓燕, 吴斌, 殷耀, 杨雯筌, 沈崇钰, 丁涛, 陈惠兰   

  1. 江苏出入境检验检疫局动植物与食品检测中心 国家蜂产品基准实验室, 江苏 南京 210001
  • 收稿日期:2012-06-21 修回日期:2012-07-25 出版日期:2012-10-28 发布日期:2012-10-17
  • 通讯作者: 许蔚,助理工程师,主要从事蜂产品中的各类抗生素分析. Tel: (025)52345187, E-mail: Cathy_xuwei@163.com.

Determination of amoxicillin in honey by high performance liquid chromatography-tandem mass spectrometry

XU Wei*, ZHANG Xiaoyan, WU Bin, YIN Yao, YANG Wenquan, SHEN Chongyu, DING Tao, CHEN Huilan   

  1. National Honey Reference Laboratory, Animal, Plant and Food Inspection Center (APFIC) of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • Received:2012-06-21 Revised:2012-07-25 Online:2012-10-28 Published:2012-10-17

PDF

379

被引次数

29

摘要： 建立了高效液相色谱-串联质谱测定蜂蜜中阿莫西林残留的方法。样品用磷酸氢二钾溶液提取,经固相萃取柱进行净化提取后,以C18柱为分离柱,甲醇和0.1%(v/v)甲酸水溶液为流动相,用串联质谱仪检测,选择1个母离子和2个子离子进行选择反应监测,选择信号最强的子离子进行定量测定。该方法采用外标法定量,在2.0～100.0 μg/L范围内,阿莫西林的峰面积与其质量浓度呈良好的线性关系(r2＞0.99),方法的检出限和定量限分别为2.0 μg/kg和5.0 μg/kg,回收率范围为74.2%～81.7%,日内精密度范围为2.8%～7.8%,日间精密度范围为9.1%～11.3%。该方法简便快捷,可以用于蜂蜜中阿莫西林残留量的测定。

关键词: 阿莫西林, 蜂蜜, 高效液相色谱-串联质谱, 固相萃取

Abstract: A method for the determination of amoxicillin in honey by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established. The samples were dissolved by phosphate buffer and cleaned-up by solid phase extraction (SPE) cartridge. The analytes were determined by HPLC-MS/MS on a C18 column with methanol and 0.1% (v/v) formic acid solution as mobile phases with gradient elution. The analysis of amoxicillin was performed under selected reaction monitoring mode by selecting one parent ion and two daughter ions as qualitative ions and the most abundant daughter ion as quantitative ion. The external standard was used for quantitative analysis in this method. The calibration curve showed good linearity in the range of 2.0~100.0 μg/L with good precision and accuracy (r2＞0.99). The limit of detection (LOD) and limit of quantitation (LOQ) were 2.0 μg/kg and 5.0 μg/kg, respectively. The average recoveries of amoxicillin in spiked honey ranged from 74.2% to 81.7% with the intra-day precisions (relative standard deviations, RSDs) from 2.8% to 7.8% and the inter-day precisions (RSDs) from 9.1% to 11.3%. This method is convenient and suitable for the determination of amoxicillin in honey.

Key words: amoxicillin, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), honey, solid phase extraction (SPE)