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—0．05mg／L范围内与其峰面积具有良好的线性关系，检测低限均为20ug／kg，3个加标水平（每种抗生素的添加水平均为20，100和200ug／kg）下的加标回收率为73．0％～90．2％，相对标准偏差为5．6％～10．5％。
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 C18c olumn. 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 ug/kg. The recoveries were between 73.0% -90.2% at three spiked levels （20, 100 and 200 ug/kg for each macrolide antibiotic）, and the relative standard deviations were between 5. 6% - 10. 5%.
出处
《色谱》
CAS
CSCD
北大核心
2007年第3期404-407,共4页
Chinese Journal of Chromatography
基金
国家质量监督检验检疫总局课题(No.2006IK117)
关键词
高效液相色谱-质谱/质谱法
大环内酯类抗生素残留
蜂王浆
high performance liquid chromatography tandem mass spectrometry （ HPLC-MS/ MS）
macrolide antibiotic residues
royal jelly
作者简介
通讯联系人：谢文，女，高级工程师，Tel：（0571）89955357，E-mail：xw@ziq．gov.cn．
