摘要
采用高效液相色谱-串联质谱(HPLC—MS/MS)法同时测定了蜂王浆中氯霉素、甲砜霉素和氟甲砜霉素残留。样品加入阴性蜂蜜和水均质后,采用乙酸乙酯提取,蒸发浓缩,C18固相萃取净化。HPLC分离后,串联质谱法以电喷雾负离子多反应监测方式(MRM)进行定性定量分析。通过对固相萃取条件的优化,大大减小了基质的干扰。氯霉素、氟甲砜霉素和甲砜霉素的检出限分别为0.1ng/g、0.2ng/g和0.5ng/g,平均回收率为89.9%~98.4%,相对标准偏差(RSD)均小于8.2%。
A method was presented for simultaneous determination of residues of chloramphenicol (CAP), thiamphenicol (TAP) and florfenicol (FF) in royal jelly by using high performance liquid chromatography tandem mass spectrometry (LC-MS/MS). After a preliminary homogenization with negative honey and water, samples were extracted with ethyl acetate, and evaporated to dryness; then, the clean up was carried out on a C18 SPE cartridge. In order to decrease the matrix interference, the conditions of solid phase extraction were optimized. After reversed-phase HPLC separation, identification and quantification were performed using multiple reaction monitoring (MRM) and electrospray ionization in negative mode. The detection limits for CAP,FF and TAP were 0.1 ng.g^-1 , 0.2 ng.g^-1 and 0.5 ng.g^-1, respectively with the average recoveries of 89.9%-98.4% and the RSD less than 8.2 %.
出处
《分析科学学报》
CAS
CSCD
2007年第5期527-531,共5页
Journal of Analytical Science
基金
国家自然科学基金(No.20407009)
湖北省自然科学基金(No.2003ABA060)
关键词
氯霉素
蜂王浆
固相萃取
高效液相色谱-串联质谱法
Chloramphenicol
Royal jelly
High performance Liquid chromatography-tandem mass spectrometry
作者简介
通讯联系人:梅素容,女,副教授,研究方向:卫生检验新技术.