摘要
目的建立液相色谱-串联质谱法检测蜂蜜中氯霉素残留量的方法。方法试样前处理采用液液萃取,以甲醇+水(71+29体积分数)为流动相,用Zorbax Eclipse XDB C18柱进行分离,以氘代氯霉素作为内标,采用负离子方式,液相色谱-电喷雾串联质谱法进行测定。结果平均回收率为93.0%-98.2%,相对标准偏差小于8%。采用空白蜂蜜基质制作校正曲线,蜂蜜中氯霉素检测的线性范围为0.01-1.00μg/kg,定量检测下限为0.01μg/kg。结论方法灵敏、准确、快速,能满足蜂蜜中氯霉素的监督检测。
Objective A liquid chromatography-tandem mass spectrometry method was developed for the determination of chloramphenicol （CAP） in honey. Method The analyte was extracted from honey samples by liquid-liquid extraction, separated on a Zorbax Eclipse XDB Cls column with methanol ＋ water （71 ＋ 29 V/V） as mobile phase and detected by tandem mass spectrometry with electrospray ionization source operating in negative ion mode. An isotopically labelled internal standard （d5-CAP） was used. Results The mean recoveries ranged from 93.0 % to 98.2 % and the relative standard derivations were lower than 8%. The matrix-matched calibration curve showed good linearity in the range of 0.01 ～ 1.00 μg/kg in honey samples. The limit of quantification for CAP in honey samples was 0.01 μg/kg. Conclusion The method was rapid, sensitive and specific. It is suitable for determination of CAP in honey.
出处
《中国食品卫生杂志》
2007年第2期117-119,共3页
Chinese Journal of Food Hygiene
关键词
色谱法
光谱分析
质量
氯霉素
蜂蜜
Chromatography
Spectrum Analysis, Mass
Chloramphenicol
Honey
