Ishii Rie, Horie Masakazu, Murayama Mitsunori, Maitani Tamio
Saitama Prefectural Institute of Public Health, Japan.
Shokuhin Eiseigaku Zasshi. 2006 Apr;47(2):58-65. doi: 10.3358/shokueishi.47.58.
A sensitive and selective method using liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) was developed for the determination of chloramphenicol (CAP) in honey and royal jelly. Mass spectral acquisition was performed in the negative mode by applying multiple reaction monitoring. In LC separation, Mightyl RP-18GP and 10 mmol/L ammonium acetate-acetonitrile were used as the column and mobile phase, respectively. CAP in honey samples was diluted with water, while CAP in royal jelly was extracted with 1% metaphosphoric acid-methanol (4 : 6). The solutions were cleaned up with an Oasis HLB cartridge. The quantification limits of CAP in honey and royal jelly were 0.3 ng/g and 1.5 ng/g, respectively. The recoveries of CAP from both honey and royal jelly at the quantification limits were over 92%. Twenty honey products and seven royal jelly products were analyzed by the developed method. CAP was detected in one honey product at 0.6 ng/g and in six royal jelly products at the level of 1.5-17.8 ng/g. These results show that the developed method has satisfactory sensitivity selectivity and is useful for the determination of CAP residues in honey and royal jelly.
建立了一种采用液相色谱-电喷雾电离串联质谱(LC-ESI-MS/MS)测定蜂蜜和蜂王浆中氯霉素(CAP)的灵敏且选择性好的方法。通过多反应监测在负离子模式下进行质谱采集。在液相色谱分离中,分别使用Mightyl RP-18GP柱和10 mmol/L乙酸铵-乙腈作为流动相。蜂蜜样品中的CAP用水稀释,而蜂王浆中的CAP用1%偏磷酸-甲醇(4:6)提取。溶液用Oasis HLB柱净化。蜂蜜和蜂王浆中CAP的定量限分别为0.3 ng/g和1.5 ng/g。在定量限水平,蜂蜜和蜂王浆中CAP的回收率均超过92%。采用所建立的方法对20种蜂蜜产品和7种蜂王浆产品进行了分析。在一种蜂蜜产品中检测到CAP含量为0.6 ng/g,在6种蜂王浆产品中检测到CAP含量为1.5 - 17.8 ng/g。这些结果表明,所建立的方法具有令人满意的灵敏度和选择性,可用于测定蜂蜜和蜂王浆中的CAP残留。