色谱

色谱

• 研究论文 • 上一篇    下一篇

蜂王浆产品中5种大环内酯类抗生素残留量的高效液相色谱-质谱/质谱检测方法

谢文1,丁慧瑛1,奚君阳2,钱艳2,黄雷芳2

  

  1. 1.Zhejiang Entry-Exit Inspection and Quarantine Bureau, Hangzhou 310012, China; 2.Zhejiang Lead Product Technic CO., Ltd., Hangzhou 310012, China
  • 收稿日期:2006-09-12 修回日期:2007-01-30 出版日期:2007-05-30 发布日期:1985-09-25
  • 通讯作者: 谢文

Determination of Five Macrolide Antibiotic Residues in Royal Jelly Samples by Using High Performance
Liquid Chromatography Tandem Mass Spectrometry

XIE Wen1, DING Huiying1, XI Junyang2, QIAN Yan2, HUANG Leifang2   

  1. 1.Zhejiang Entry-Exit Inspection and Quarantine Bureau, Hangzhou 310012, China; 2.Zhejiang Lead Product Technic CO., Ltd., Hangzhou 310012, China
  • Received:2006-09-12 Revised:2007-01-30 Online:2007-05-30 Published:1985-09-25

PDF

893

摘要：

建立了高效液相色谱-质谱/质谱测定蜂王浆中5种大环内酯类抗生素(螺旋霉素、竹桃霉素、泰乐菌素、罗红霉素、交沙霉素)残留的方法。先用三氯乙酸沉淀蜂王浆中的蛋白质，上层清液再用乙腈提取、C18小柱净化。每种抗生素选择一个母离子和两个子离子进行监测。5种大环内酯类抗生素在0.002～0.05 mg/L 范围内与其峰面积具有良好的线性关系,检测低限均为20 μg/kg,3个加标水平（每种抗生素的添加水平均为20, 100 和 200 μg/kg）下的加标回收率为73.0%～90.2%,相对标准偏差为5.6%～10.5%。

关键词: 大环内酯类抗生素残留, 蜂王浆
, 高效液相色谱-质谱/质谱法

Abstract:

The macrolides are lipophilic molecules having a central lactone ring bearing 12 to 20 atoms to which several amino and/or neutral sugars are bound. They are broad spectrum antibiotics active against Gram-positive bacteria and mycoplasmas, as well as some Gram-negative organisms and members of the chlamydia group. Macrolides are a group of antibacterial compounds that have been widely used in medical and veterinary practices. A method of high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was developed for the confirmation of five macrolide antibiotic residues (spiramycin, oleandomycin, tylosin, roxithromycin, josamycin) in royal jelly samples. Trichloroacetic acid solution was used to precipitate the protein in the sample. The upper layer solution was extracted with acetonitrile. Then it was cleaned up with a C18 column. The one precursor/two product ion transitions for each macrolide antibiotics were monitored. The results show that the working curves for five macrolide antibiotics were linear in the range of 0.002-0.05 mg/L by HPLC-MS/MS in selective ion monitoring model. The limits of quantitation of the antibiotics in royal jelly were all 20 μg/kg. The recoveries were between 73.0%-90.2% at three spiked levels （20, 100 and 200 μg/kg for each macrolide antibiotic）, and the relative standard deviations were between 5.6%-10.5%.

Key words: macrolide antibiotic residues, royal jelly , high performance liquid chromatography tandem mass spectrometry （HPLC-MS/MS）